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Binding Models and Theory

Filip Hládek edited this page Oct 10, 2025 · 1 revision

Binding Models and Theory

This page documents the mathematical foundation and thermodynamic models used in BEAST. Each model represents a different chemical equilibrium scenario commonly encountered in NMR titration studies of host-guest systems.

For complete mathematical derivations, see Model Proofs section below the general notes.


General Notation

Concentrations

  • $[H_0]$: Total host concentration (mol/L)
  • $[G_0]$: Total guest concentration (mol/L)
  • $[H]$: Free (unbound) host concentration
  • $[G]$: Free (unbound) guest concentration
  • $[HG]$, $[HG_2]$, $[H_2G]$, $[H_2]$: Complex concentrations

Equilibrium Constants

  • $K_{HG}$: Association constant for H + G ⇌ HG (M⁻¹)
  • $K_{HG_2}$ or $K_d$: Association constant for HG + G ⇌ HG₂ (M⁻¹)
  • $K_{H_2G}$: Association constant for H + HG ⇌ H₂G (M⁻¹)
  • $K_{H_2}$ or $K_d$: Dimerization constant for 2H ⇌ H₂ (M⁻¹)

Chemical Shifts

  • $\delta_{obs}$: Observed chemical shift (Hz or ppm)
  • $\delta_{free}$ or $\delta_G$: Chemical shift of free guest (reference = 0)
  • $\Delta\delta$: Chemical shift change relative to free guest
  • $d_{inf}$, $d_{HG}$, $d_{H_2G}$: Limiting chemical shifts of bound species

Important Notes

  • All models assume guest-observed NMR (monitoring guest signal)
  • Chemical shifts of free guest serve as the reference point (Δδ = 0)
  • Only species containing guest molecules contribute to the observed shift
  • Fast exchange on the NMR timescale is assumed (population-weighted average)

Model 1: 1:1 Host-Guest Binding (HG)

Equilibrium

$$H + G \rightleftharpoons HG$$

$$K_{HG} = \frac{[HG]}{[H][G]}$$

Description

The simplest binding scenario where one host molecule binds to one guest molecule to form a 1:1 complex. This is the most common binding mode in supramolecular chemistry.

Algebraic Solution

Mass balance equations:

$$[H_0] = [H] + [HG]$$ $$[G_0] = [G] + [HG]$$

Quadratic equation solution:

$$[HG] = \frac{1}{2}\left([H_0] + [G_0] + \frac{1}{K_{HG}} - \sqrt{\left([H_0] + [G_0] + \frac{1}{K_{HG}}\right)^2 - 4[H_0][G_0]}\right)$$

Chemical Shift Calculation

$$\Delta\delta = d_{inf} \cdot \frac{[HG]}{[G_0]}$$

Fitted Parameters

  • $K_{HG}$: Binding constant (M⁻¹)
  • $d_{inf}$: Limiting chemical shift of bound guest (Hz or ppm)

Physical Interpretation

  • Strong binding: $K_{HG} > 10^5$ M⁻¹
  • Moderate binding: $10^3 < K_{HG} < 10^5$ M⁻¹
  • Weak binding: $K_{HG} < 10^3$ M⁻¹

Model 2: 1:2 Host-Guest Binding (HG + HG₂)

Equilibria

$$H + G \rightleftharpoons HG \quad (K_{HG})$$ $$HG + G \rightleftharpoons HG_2 \quad (K_{HG_2})$$

Description

Sequential binding of two guests to one host molecule. The first guest binds with constant $K_{HG}$, and the second guest binds to the resulting HG complex with constant $K_{HG_2}$ (also called $K_d$).

Algebraic Solution

Cubic equation for free guest concentration [G]:

$$a[G]^3 + b[G]^2 + c[G] + d = 0$$

Where:

  • $a = K_{HG} \cdot K_{HG_2}$
  • $b = K_{HG}(2K_{HG_2}[H_0] - K_{HG_2}[G_0] + 1)$
  • $c = K_{HG}([H_0] - [G_0]) + 1$
  • $d = -[G_0]$

Solution method: Select the smallest positive real root.

Complex concentrations:

$$[HG] = \frac{K_{HG}[H_0][G]}{1 + K_{HG}[G] + K_{HG}K_{HG_2}[G]^2}$$

$$[HG_2] = \frac{K_{HG}K_{HG_2}[H_0][G]^2}{1 + K_{HG}[G] + K_{HG}K_{HG_2}[G]^2}$$

Chemical Shift Calculation

$$\Delta\delta = \frac{d_{HG} \cdot [HG] + d_{HG_2} \cdot 2[HG_2]}{[G_0]}$$

Note: Factor of 2 for $[HG_2]$ accounts for two guest molecules per complex.

Fitted Parameters

  • $K_{HG}$: First binding constant (M⁻¹)
  • $K_{HG_2}$: Second binding constant (M⁻¹)
  • $d_{HG}$: Chemical shift of guest in HG
  • $d_{HG_2}$: Chemical shift of guest in HG₂

Cooperativity Analysis

  • Positive cooperativity: $K_{HG_2} > K_{HG}$ (second guest binds stronger)
  • Negative cooperativity: $K_{HG_2} < K_{HG}$ (second guest binds weaker)
  • Non-cooperative: $K_{HG_2} \approx K_{HG}$

Model 3: 2:1 Host-Guest Binding (HG + H₂G)

Equilibria

$$H + G \rightleftharpoons HG \quad (K_{HG})$$ $$H + HG \rightleftharpoons H_2G \quad (K_{H_2G})$$

Description

Sequential binding of two hosts to one guest molecule. First, HG forms with constant $K_{HG}$, then a second host binds to form H₂G with constant $K_{H_2G}$ (also called $K_d$).

Algebraic Solution

Cubic equation for free host concentration [H]:

$$a[H]^3 + b[H]^2 + c[H] + d = 0$$

Where:

  • $a = K_{HG} \cdot K_{H_2G}$
  • $b = K_{HG}(2K_{H_2G}[G_0] - K_{H_2G}[H_0] + 1)$
  • $c = K_{HG}([G_0] - [H_0]) + 1$
  • $d = -[H_0]$

Solution method: Select the smallest positive real root.

Complex concentrations:

$$[HG] = \frac{K_{HG}[H][G_0]}{1 + K_{HG}[H] + K_{HG}K_{H_2G}[H]^2}$$

$$[H_2G] = \frac{K_{HG}K_{H_2G}[H]^2[G_0]}{1 + K_{HG}[H] + K_{HG}K_{H_2G}[H]^2}$$

Chemical Shift Calculation

$$\Delta\delta = \frac{d_{HG} \cdot [HG] + d_{H_2G} \cdot [H_2G]}{[G_0]}$$

Fitted Parameters

  • $K_{HG}$: First binding constant (M⁻¹)
  • $K_{H_2G}$: Second binding constant (M⁻¹)
  • $d_{HG}$: Chemical shift of guest in HG
  • $d_{H_2G}$: Chemical shift of guest in H₂G

Physical Interpretation

This model is common when:

  • Host molecules can aggregate around the guest
  • Guest acts as a template for host assembly
  • Sandwich complexes form in supramolecular systems

Model 4: Host Dimerization with Guest Binding (HG + H₂)

Equilibria

$$H + G \rightleftharpoons HG \quad (K_{HG})$$ $$2H \rightleftharpoons H_2 \quad (K_{H_2})$$

Description

Competitive equilibria where host-guest binding occurs simultaneously with host self-association (dimerization). The host dimer (H₂) does not bind guest in this model.

Algebraic Solution

Cubic equation for free host concentration [H]:

$$a[H]^3 + b[H]^2 + c[H] + d = 0$$

Where:

  • $a = 2K_{HG}K_{H_2}$
  • $b = K_{HG} + 2K_{H_2}$
  • $c = K_{HG}([G_0] - [H_0]) + 1$
  • $d = -[H_0]$

Solution method: Select the smallest positive real root.

Free guest concentration:

$$[G] = \frac{[G_0]}{1 + K_{HG}[H]}$$

Complex concentrations:

$$[HG] = \frac{K_{HG}[H][G_0]}{1 + K_{HG}[H]}$$

$$[H_2] = K_{H_2}[H]^2$$

Chemical Shift Calculation

$$\Delta\delta = \frac{d_{HG} \cdot [HG]}{[G_0]}$$

Note: H₂ does not contain guest, so it doesn't contribute to guest-observed shift.

Fitted Parameters

  • $K_{HG}$: Host-guest binding constant (M⁻¹)
  • $K_{H_2}$: Host dimerization constant (M⁻¹)
  • $d_{HG}$: Chemical shift of guest in HG complex

Physical Interpretation

This model applies when:

  • Host molecules tend to self-associate in solution
  • Dimerization competes with guest binding
  • Higher host concentrations reduce apparent binding affinity
  • Common in systems with π-π stacking or hydrogen bonding hosts

Model 5: Multi-Equilibrium System (HG + H₂ + H₂G)

Equilibria

$$H + G \rightleftharpoons HG \quad (K_{HG})$$ $$2H \rightleftharpoons H_2 \quad (K_{H_2})$$ $$H + HG \rightleftharpoons H_2G \quad (K_{H_2G})$$

Description

Complex system with three competing equilibria: 1:1 binding, host dimerization, and 2:1 complex formation. This is the most general model and can describe systems where multiple processes occur simultaneously.

Algebraic Solution

Iterative numerical solution required due to quartic polynomial complexity.

Mass balance equations:

$$[H_0] = [H] + [HG] + 2[H_2] + 2[H_2G]$$ $$[G_0] = [G] + [HG] + [H_2G]$$

Iterative scheme:

  1. Initial guess: $[H]_0$, $[G]_0$
  2. Calculate complexes:
    • $[HG] = K_{HG}[H][G]$
    • $[H_2] = K_{H_2}[H]^2$
    • $[H_2G] = K_{H_2G}K_{HG}[H]^2[G]$
  3. Update free concentrations from mass balance
  4. Repeat until convergence (typically $|\Delta[H]| < 10^{-6}$)

Chemical Shift Calculation

For guest-observed NMR, only HG and H₂G contribute:

$$\Delta\delta = \frac{d_{HG} \cdot [HG] + d_{H_2G} \cdot [H_2G]}{[G_0]}$$

Note: H₂ doesn't contribute (no guest molecule).

Fitted Parameters

  • $K_{HG}$: Host-guest binding constant (M⁻¹)
  • $K_{H_2}$: Host dimerization constant (M⁻¹)
  • $K_{H_2G}$: Second host binding constant (M⁻¹)
  • $d_{HG}$: Chemical shift of guest in HG
  • $d_{H_2G}$: Chemical shift of guest in H₂G

Thermodynamic Relationships

The overall formation of H₂G can occur via:

Sequential pathway: $$2H + G \rightleftharpoons H_2G \quad K_{overall} = K_{HG} \times K_{H_2G}$$

This model is particularly relevant when:

  • Host aggregation is significant
  • Multiple binding modes coexist
  • Concentration-dependent behavior is observed
  • Simple models fail to fit the data adequately

Model Selection Guidelines

When to Use Each Model

Model Use When
1:1 (HG) Simple binding curve, clear saturation, no evidence of higher-order complexes
1:2 (HG + HG₂) Two distinct binding regions, biphasic curve, guest in excess
2:1 (HG + H₂G) Binding increases with host concentration, evidence of sandwich complexes
Dimer (HG + H₂) Non-linear behavior at high host concentration, aggregation-prone hosts
Multi (HG + H₂ + H₂G) Complex behavior, multiple equilibria evident, simple models fail

Model Comparison Criteria

BEAST automatically fits all models and ranks them using:

  • AIC (Akaike Information Criterion) - Penalizes complexity
  • BIC (Bayesian Information Criterion) - More stringent penalty
  • - Goodness of fit
  • Residual diagnostics - Systematic patterns indicate wrong model

Lower AIC/BIC = Better model


Numerical Considerations

Root Selection for Polynomial Equations

When solving cubic equations for [G] or [H]:

  1. Calculate all roots (may be complex)
  2. Filter for real roots
  3. Filter for positive roots
  4. Select smallest positive root within physical bounds:
    • $0 < [G] \leq [G_0]$
    • $0 < [H] \leq [H_0]$

Fallback Strategy

If no valid root is found (rare, usually during initial guess optimization):

  • Set $[H] \approx 10^{-10}$ M or $[G] \approx 10^{-10}$ M
  • Prevents division by zero
  • Allows optimization to continue toward valid parameter space

Convergence Criteria (Multi-Equilibrium Model)

Iterative solution converges when: $$|\Delta[H]| < 10^{-6} \text{ and } |\Delta[G]| < 10^{-6}$$

Maximum iterations: 100,000 (typically converges in < 100)


Chemical Shift Fundamentals

Population-Weighted Average

The observed chemical shift is the mole-fraction-weighted average of all species:

$$\delta_{obs} = \sum_i \frac{\delta_i \cdot [species_i]}{[total]}$$

Delta-Delta (Δδ) Convention

Chemical shift changes are reported relative to free guest:

$$\Delta\delta = \delta_{obs} - \delta_{free}$$

Since $\delta_{free} = 0$ (reference point):

$$\Delta\delta = \frac{\sum_i \delta_i \cdot [G_{in\ complex_i}]}{[G_0]}$$

This explains why:

  • $\Delta\delta = 0$ when no binding occurs
  • $\Delta\delta$ increases toward $d_{inf}$ at saturation
  • Units are Hz or ppm depending on input data

Implementation Notes

Units

  • Concentrations: mol/L (M)
  • Chemical shifts: Hz or ppm (consistent with input)
  • Association constants: M⁻¹

Assumptions

  1. Fast exchange on NMR timescale (averaged signal)
  2. Guest-observed NMR (monitoring guest nucleus)
  3. No guest aggregation (only host-guest complexes)
  4. Closed system (no precipitation or phase separation)
  5. Temperature-independent K during measurement

Limitations

  • Cannot distinguish between different binding geometries with same stoichiometry
  • Requires sufficient data points (≥8-10) for reliable fitting
  • Multiple models may fit data equally well (use AIC/BIC for selection)
  • Extreme affinity ($K &gt; 10^8$ M⁻¹) may be difficult to measure accurately

Mathematical Derivations of Binding Isotherm Models

This section provides detailed mathematical derivations for the 1:1, 1:2, and 2:1 host-guest binding models used in BEAST (Binding Evaluation and Analysis Software Tool).


1:1 Host-Guest Binding Model

Equilibrium Expression

The simplest binding model describes the formation of a 1:1 complex between host (H) and guest (G):

$$H + G \rightleftharpoons HG$$

Equilibrium constant:

$$K_{HG} = \frac{[HG]}{[H][G]}$$

Mass Balance Equations

Total host concentration:

$$[H_0] = [H] + [HG]$$

Total guest concentration:

$$[G_0] = [G] + [HG]$$

Algebraic Solution

From the mass balance equations:

$$[H] = [H_0] - [HG]$$ $$[G] = [G_0] - [HG]$$

Substituting into the equilibrium expression:

$$K_{HG} = \frac{[HG]}{([H_0] - [HG])([G_0] - [HG])}$$

Rearranging:

$$K_{HG}([H_0] - [HG])([G_0] - [HG]) = [HG]$$

Expanding:

$$K_{HG}([H_0][G_0] - [H_0][HG] - [G_0][HG] + [HG]^2) = [HG]$$

$$K_{HG}[H_0][G_0] - K_{HG}[H_0][HG] - K_{HG}[G_0][HG] + K_{HG}[HG]^2 = [HG]$$

Rearranging into standard quadratic form:

$$K_{HG}[HG]^2 - (K_{HG}[H_0] + K_{HG}[G_0] + 1)[HG] + K_{HG}[H_0][G_0] = 0$$

Dividing by $K_{HG}$:

$$[HG]^2 - ([H_0] + [G_0] + \frac{1}{K_{HG}})[HG] + [H_0][G_0] = 0$$

Quadratic formula solution:

$$[HG] = \frac{([H_0] + [G_0] + \frac{1}{K_{HG}}) \pm \sqrt{([H_0] + [G_0] + \frac{1}{K_{HG}})^2 - 4[H_0][G_0]}}{2}$$


1:2 Host-Guest Binding Model

Equilibrium Expressions

This model describes sequential binding of two guests to one host:

$$H + G \rightleftharpoons HG \quad (K_{HG})$$ $$HG + G \rightleftharpoons HG_2 \quad (K_{HG_2})$$

Equilibrium constants:

$$K_{HG} = \frac{[HG]}{[H][G]}$$ $$K_{HG_2} = \frac{[HG_2]}{[HG][G]}$$

Mass Balance Equations

Total host concentration:

$$[H_0] = [H] + [HG] + [HG_2]$$

Total guest concentration:

$$[G_0] = [G] + [HG] + 2[HG_2]$$

Algebraic Solution

From the equilibrium expressions:

$$[HG] = K_{HG}[H][G]$$ $$[HG_2] = K_{HG_2}[HG][G] = K_{HG} K_{HG_2}[H][G]^2$$

From host mass balance:

$$[H_0] = [H] + K_{HG}[H][G] + K_{HG} K_{HG_2}[H][G]^2$$ $$[H_0] = [H](1 + K_{HG}[G] + K_{HG} K_{HG_2}[G]^2)$$

Therefore:

$$[H] = \frac{[H_0]}{1 + K_{HG}[G] + K_{HG} K_{HG_2}[G]^2}$$

Substituting back:

$$[HG] = \frac{K_{HG}[H_0][G]}{1 + K_{HG}[G] + K_{HG} K_{HG_2}[G]^2}$$ $$[HG_2] = \frac{K_{HG} K_{HG_2}[H_0][G]^2}{1 + K_{HG}[G] + K_{HG} K_{HG_2}[G]^2}$$

From guest mass balance:

$$[G_0] = [G] + \frac{K_{HG}[H_0][G]}{1 + K_{HG}[G] + K_{HG} K_{HG_2}[G]^2} + 2\frac{K_{HG} K_{HG_2}[H_0][G]^2}{1 + K_{HG}[G] + K_{HG} K_{HG_2}[G]^2}$$

Multiplying through by the denominator:

$$[G_0](1 + K_{HG}[G] + K_{HG} K_{HG_2}[G]^2) = [G](1 + K_{HG}[G] + K_{HG} K_{HG_2}[G]^2) + K_{HG}[H_0][G] + 2K_{HG} K_{HG_2}[H_0][G]^2$$

Rearranging:

$$[G_0] + [G_0]K_{HG}[G] + [G_0]K_{HG} K_{HG_2}[G]^2 = [G] + K_{HG}[G]^2 + K_{HG} K_{HG_2}[G]^3 + K_{HG}[H_0][G] + 2K_{HG} K_{HG_2}[H_0][G]^2$$

Collecting terms:

$$K_{HG} K_{HG_2}[G]^3 + K_{HG}(2K_{HG_2}[H_0] - K_{HG_2}[G_0] + 1)[G]^2 + (K_{HG}([H_0] - [G_0])+1)[G] - ([G_0]) = 0$$

Cubic equation in [G] (free guest concentration):

$$a[G]^3 + b[G]^2 + c[G] + d = 0$$

Where:

  • $a = K_{HG} K_{HG_2}$
  • $b = K_{HG}(2K_{HG_2}[H_0] - K_{HG_2}[G_0] + 1)$
  • $c = K_{HG}([H_0] - [G_0]) + 1$
  • $d = -[G_0]$

2:1 Host-Guest Binding Model

Equilibrium Expressions

This model describes sequential binding of two hosts to one guest:

$$H + G \rightleftharpoons HG \quad (K_{HG})$$ $$H + HG \rightleftharpoons H_2G \quad (K_{H_2G})$$

Equilibrium constants:

$$K_{HG} = \frac{[HG]}{[H][G]}$$ $$K_{H_2G} = \frac{[H_2G]}{[H][HG]}$$

Mass Balance Equations

Total host concentration:

$$[H_0] = [H] + [HG] + 2[H_2G]$$

Total guest concentration:

$$[G_0] = [G] + [HG] + [H_2G]$$

Algebraic Solution

From the equilibrium expressions:

$$[HG] = K_{HG}[H][G]$$ $$[H_2G] = K_{H_2G}[H][HG] = K_{HG} K_{H_2G}[H]^2[G]$$

From guest mass balance:

$$[G_0] = [G] + K_{HG}[H][G] + K_{HG} K_{H_2G}[H]^2[G]$$ $$[G_0] = [G](1 + K_{HG}[H] + K_{HG} K_{H_2G}[H]^2)$$

Therefore:

$$[G] = \frac{[G_0]}{1 + K_{HG}[H] + K_{HG} K_{H_2G}[H]^2}$$

Substituting back:

$$[HG] = \frac{K_{HG}[H][G_0]}{1 + K_{HG}[H] + K_{HG} K_{H_2G}[H]^2}$$ $$[H_2G] = \frac{K_{HG} K_{H_2G}[H]^2[G_0]}{1 + K_{HG}[H] + K_{HG} K_{H_2G}[H]^2}$$

From host mass balance:

$$[H_0] = [H] + \frac{K_{HG}[H][G_0]}{1 + K_{HG}[H] + K_{HG} K_{H_2G}[H]^2} + 2\frac{K_{HG} K_{H_2G}[H]^2[G_0]}{1 + K_{HG}[H] + K_{HG} K_{H_2G}[H]^2}$$

Multiplying through by the denominator:

$$[H_0](1 + K_{HG}[H] + K_{HG} K_{H_2G}[H]^2) = [H](1 + K_{HG}[H] + K_{HG} K_{H_2G}[H]^2) + K_{HG}[H][G_0] + 2K_{HG} K_{H_2G}[H]^2[G_0]$$

Rearranging:

$$[H_0] + [H_0]K_{HG}[H] + [H_0]K_{HG} K_{H_2G}[H]^2 = [H] + K_{HG}[H]^2 + K_{HG} K_{H_2G}[H]^3 + K_{HG}[G_0][H] + 2K_{HG} K_{H_2G}[G_0][H]^2$$

Collecting terms:

$$K_{HG} K_{H_2G}[H]^3 + K_{HG}(2K_{H_2G}[G_0] - K_{H_2G}[H_0] + 1)[H]^2 + (K_{HG}([G_0] - [H_0])+1)[H] - ([H_0]) = 0$$

Cubic equation in [H] (free host concentration):

$$a[H]^3 + b[H]^2 + c[H] + d = 0$$

Where:

  • $a = K_{HG} K_{H_2G}$
  • $b = K_{HG}(2K_{H_2G}[G_0] - K_{H_2G}[H_0] + 1)$
  • $c = K_{HG}([G_0] - [H_0]) + 1$
  • $d = -[H_0]$

Host Dimerization Model (HG + H₂)

Equilibrium Expressions

This model describes host-guest binding in competition with host dimerization:

$$H + G \rightleftharpoons HG \quad (K_{HG})$$ $$2H \rightleftharpoons H_2 \quad (K_{H_2})$$

Equilibrium constants:

$$K_{HG} = \frac{[HG]}{[H][G]}$$ $$K_{H_2} = \frac{[H_2]}{[H]^2}$$

Mass Balance Equations

Total host concentration:

$$[H_0] = [H] + [HG] + 2[H_2]$$

Total guest concentration:

$$[G_0] = [G] + [HG]$$

Algebraic Solution

From the equilibrium expressions:

$$[HG] = K_{HG}[H][G]$$ $$[H_2] = K_{H_2}[H]^2$$

From guest mass balance:

$$[G_0] = [G] + K_{HG}[H][G]$$ $$[G_0] = [G](1 + K_{HG}[H])$$

Therefore:

$$[G] = \frac{[G_0]}{1 + K_{HG}[H]}$$

Substituting back:

$$[HG] = \frac{K_{HG}[H][G_0]}{1 + K_{HG}[H]}$$

From host mass balance:

$$[H_0] = [H] + \frac{K_{HG}[H][G_0]}{1 + K_{HG}[H]} + 2K_{H_2}[H]^2$$

Multiplying through by $(1 + K_{HG}[H])$:

$$[H_0](1 + K_{HG}[H]) = [H](1 + K_{HG}[H]) + K_{HG}[H][G_0] + 2K_{H_2}[H]^2(1 + K_{HG}[H])$$

Expanding:

$$[H_0] + [H_0]K_{HG}[H] = [H] + K_{HG}[H]^2 + K_{HG}[H][G_0] + 2K_{H_2}[H]^2 + 2K_{H_2}K_{HG}[H]^3$$

Rearranging:

$$2K_{H_2}K_{HG}[H]^3 + (K_{HG} + 2K_{H_2})[H]^2 + (K_{HG}([G_0] - [H_0])+1)[H] - [H_0] = 0$$

Cubic equation in [H] (free host concentration):

$$a[H]^3 + b[H]^2 + c[H] + d = 0$$

Where:

  • $a = 2K_{HG}K_{H_2}$
  • $b = K_{HG} + 2K_{H_2}$
  • $c = K_{HG}([G_0] - [H_0]) + 1$
  • $d = -[H_0]$

Multi-Equilibrium Model (HG + H₂ + H₂G)

Equilibrium Expressions

This model describes a complex system with three competing equilibria:

$$H + G \rightleftharpoons HG \quad (K_{HG})$$ $$2H \rightleftharpoons HH_2 \quad (K_{H_2})$$ $$H + HG \rightleftharpoons H_2G \quad (K_{H_2G})$$

Equilibrium constants: $$K_{HG} = \frac{[HG]}{[H][G]}$$ $$K_{H_2} = \frac{[H_2]}{[H]^2}$$ $$K_{H_2G} = \frac{[H_2G]}{[H][HG]}$$

Mass Balance Equations

Total host concentration: $$[H_0] = [H] + [HG] + 2[H_2] + 2[H_2G]$$

Total guest concentration: $$[G_0] = [G] + [HG] + [H_2G]$$

Algebraic Solution

From the equilibrium expressions:

$$[HG] = K_{HG}[H][G]$$ $$[H_2] = K_{H_2}[H]^2$$ $$[H_2G] = K_{H_2G}[H][HG] = K_{H_2G}K_{HG}[H]^2[G]$$

From guest mass balance:

$$[G_0] = [G] + K_{HG}[H][G] + K_{H_2G}K_{HG}[H]^2[G]$$ $$[G_0] = [G](1 + K_{HG}[H] + K_{H_2G}K_{HG}[H]^2)$$

Therefore:

$$[G] = \frac{[G_0]}{1 + K_{HG}[H] + K_{H_2G}K_{HG}[H]^2}$$

Substituting back:

$$[HG] = \frac{K_{HG}[H][G_0]}{1 + K_{HG}[H] + K_{H_2G}K_{HG}[H]^2}$$ $$[H_2G] = \frac{K_{H_2G}K_{HG}[H]^2[G_0]}{1 + K_{HG}[H] + K_{H_2G}K_{HG}[H]^2}$$

From host mass balance:

$$[H_0] = [H] + \frac{K_{HG}[H][G_0]}{1 + K_{HG}[H] + K_{H_2G}K_{HG}[H]^2} + 2K_{H_2}[H]^2 + 2\frac{K_{H_2G}K_{HG}[H]^2[G_0]}{1 + K_{HG}[H] + K_{H_2G}K_{HG}[H]^2}$$

Multiplying through by the denominator:

$$[H_0](1 + K_{HG}[H] + K_{H_2G}K_{HG}[H]^2) = [H](1 + K_{HG}[H] + K_{H_2G}K_{HG}[H]^2) + K_{HG}[H][G_0] + 2K_{H_2}[H]^2(1 + K_{HG}[H] + K_{H_2G}K_{HG}[H]^2) + 2K_{H_2G}K_{HG}[H]^2[G_0]$$

Expanding and collecting terms:

$$[H_0] + [H_0]K_{HG}[H] + [H_0]K_{H_2G}K_{HG}[H]^2 = [H] + K_{HG}[H]^2 + K_{H_2G}K_{HG}[H]^3 + K_{HG}[H][G_0] + 2K_{H_2}[H]^2 + 2K_{H_2}K_{HG}[H]^3 + 2K_{H_2}K_{H_2G}K_{HG}[H]^4 + 2K_{H_2G}K_{HG}[H]^2[G_0]$$

Rearranging into polynomial form:

$$2K_{H_2}K_{H_2G}K_{HG}[H]^4 + (K_{H_2G}K_{HG} + 2K_{H_2}K_{HG})[H]^3 + (2K_{H_2} + K_{HG} + 2K_{H_2G}K_{HG}[G_0] - K_{H_2G}K_{HG}[H_0])[H]^2 + (K_{HG}[G_0] - K_{HG}[H_0] + 1)[H] - [H_0] = 0$$

This leads to a quartic polynomial equation in [H] that typically requires iterative numerical solution.

Iterative Solution Method

Due to the complexity of the algebraic solution, this system is typically solved iteratively:

  1. Initial guess: Start with reasonable estimates for [H] and [G]
  2. Calculate complexes: Use equilibrium expressions to find [HG], [H₂], [H₂G]
  3. Update free concentrations: Use mass balance equations
  4. Check convergence: Repeat until changes are below tolerance
  5. Calculate chemical shift: Use final concentrations

Chemical Shift Calculation (Guest-Observed)

For guest-observed NMR, only species containing guest molecules contribute:

$$\delta_{obs} = \frac{\delta_{G}[G] + \delta_{HG}[HG] + \delta_{H_2G}[H_2G]}{[G_0]}$$

The chemical shift change relative to free guest:

$$\Delta\delta = \delta_{obs} - \delta_G = \frac{\Delta\delta_{HG}[HG] + \Delta\delta_{H_2G}[H_2G]}{[G_0]}$$

Physical Interpretation

This model describes systems where:

  • Host-guest binding competes with host dimerization
  • Host dimers can also bind guest molecules
  • The system exhibits complex behavior depending on relative binding constants
  • Higher host concentrations can favor either HG or H₂G formation depending on the equilibrium constants
  • This model is particularly relevant for systems where host aggregation is significant

Thermodynamic Relationships

The overall equilibrium for H₂G formation can be viewed as:

$$2H + G \rightleftharpoons H_2G$$

This can occur through two pathways:

  1. Sequential pathway: $H + G \rightleftharpoons HG$, then $H + HG \rightleftharpoons H_2G$
  2. Alternative pathway: $2H \rightleftharpoons H_2$, then $H_2 + G \rightleftharpoons H_2G$ (not present in this model)

The overall constant through the sequential pathway: $K_{overall} = K_{HG} \times K_{H_2G}$

This relationship helps in understanding the relative importance of the different pathways to complex formation. The formation of H₂G is directly dependent on the availability of both free host and the HG complex.


Chemical Shift Calculations

Fundamental Principle

The observed chemical shift in NMR is the population-weighted average of all species:

$$\delta_{obs} = \frac{\sum_i \delta_i [species_i]}{[total]}$$

For guest-observed experiments:

$$\delta_{obs} = \frac{\delta_{free}[G_{free}] + \delta_{HG}[G_{in_HG}] + \delta_{complex}[G_{in_complex}]}{[G_0]}$$

Delta-Delta (Δδ) Calculation

Chemical shift changes are calculated relative to the free state:

$$\Delta\delta = \delta_{obs} - \delta_{free}$$

Since $\delta_{free}$ serves as the reference (zero point):

$$\Delta\delta = \frac{\Delta\delta_{HG}[G_{in_HG}] + \Delta\delta_{complex}[G_{in_complex}]}{[G_0]}$$

Model-Specific Implementations

1:1 & Host Dimerization Models

  • Guest molecules: $[G_{\text{free}}]$ and $[G_{\text{in HG}}] = [HG]$
  • $\Delta\delta = \frac{\Delta\delta_{\text{inf}} \cdot [HG]}{[G_0]}$

1:2 Model

  • Guest molecules: $[G_{\text{free}}]$, $[G_{\text{in HG}}] = [HG]$, and $[G_{\text{in HG}_2}] = 2[HG_2]$
  • $\Delta\delta = \frac{\Delta\delta_{\text{inf1}} \cdot [HG] + \Delta\delta_{\text{inf2}} \cdot 2[HG_2]}{[G_0]}$

2:1 & Multi-Equilibrium Models

  • Guest molecules: $[G_{\text{free}}]$, $[G_{\text{in HG}}] = [HG]$, and $[G_{\text{in H}_2\text{G}}] = [H_2G]$
  • $\Delta\delta = \frac{\Delta\delta_{\text{inf1}} \cdot [HG] + \Delta\delta_{\text{inf2}} \cdot [H_2G]}{[G_0]}$

References

  1. Fielding, L. Determination of association constants (Ka) from solution NMR data. Tetrahedron 2000, 56, 6151-6170. DOI

  2. Hirose, K. A practical guide for the determination of binding constants. J. Incl. Phenom. Macrocycl. Chem. 2001, 39, 193-209. DOI

  3. Connors, K.A. Binding Constants: The Measurement of Molecular Complex Stability. John Wiley & Sons: New York, 1987. DOI

  4. Thordarson, P. Determining association constants from titration experiments in supramolecular chemistry. Chem. Soc. 2011, 40. DOI

  5. Ulatowski, F.; et. al. Recognizing the Limited Applicability of Job Plots in Studying Host–Guest Interactions in Supramolecular Chemistry. J. Org. Chem. 2016, 81, 1746-1756. DOI


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