Manipulating metal-ligand binding in allosteric coordination complexes through ring strain.
Hu, Yiming; Wang, Fiona Yihan; Xie, Yi; Coleman, Benjamin D.; Stern, Charlotte L.; Mirkin, Chad A.; Chemical communications (Cambridge, England) 61 (2025) 1906–1909; doi:10.1039/d4cc06135g

data_7134154
_publ_section_title
;
 Manipulating metal-ligand binding in allosteric coordination complexes
 through ring strain.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1906
_journal_page_last               1909
_journal_paper_doi               10.1039/d4cc06135g
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C29 H31 Cl N4 P Pt S, B F4'
_chemical_formula_sum            'C29 H31 B Cl F4 N4 P Pt S'
_chemical_formula_weight         815.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-09-18 deposited with the CCDC.	2025-01-01 downloaded from the CCDC.
;
_cell_angle_alpha                95.5090(10)
_cell_angle_beta                 100.6030(10)
_cell_angle_gamma                112.4480(10)
_cell_formula_units_Z            2
_cell_length_a                   9.19990(10)
_cell_length_b                   10.8797(2)
_cell_length_c                   20.6779(3)
_cell_measurement_reflns_used    41955
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      34.0830
_cell_measurement_theta_min      2.4520
_cell_volume                     1848.45(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -30.00  18.00   0.50    8.00    --  -12.68 -95.00 150.00   96
  2  \w    -44.00  31.00   0.50    8.00    --  -12.68  95.00 -99.00  150
  3  \w    -31.00  45.00   0.50    8.00    --   13.93 -95.00 150.00  152
  4  \w    -67.00 -19.00   0.50    8.00    --  -12.68 137.00-166.23   96
  5  \w    -88.00   0.00   0.50    8.00    --  -12.68 -19.00 -30.00  176
  6  \w    -35.00  60.00   0.50    8.00    --  -12.68  77.00 -30.00  190
  7  \w    -85.00  10.00   0.50    8.00    --  -12.68 -77.00  60.00  190
  8  \w    -86.00   0.00   0.50    8.00    --  -12.68 -37.00 -90.00  172
  9  \w    -66.00 -18.00   0.50    8.00    --  -12.68 135.00 165.90   96
 10  \w    -66.00 -18.00   0.50    8.00    --  -12.68 135.00 119.67   96
 11  \w    -24.00  21.00   0.50    8.00    --  -12.68 -99.00  90.00   90
 12  \w    -67.00 -19.00   0.50    8.00    --  -12.68 137.00  27.72   96
 13  \w    -58.00  37.00   0.50    8.00    --   13.93 -77.00  60.00  190
 14  \w     -1.00  86.00   0.50    8.00    --   13.93  57.00-120.00  174
 15  \w    -60.00   5.00   0.50    8.00    --   13.93 -19.00 120.00  130
 16  \w      2.00  87.00   0.50    8.00    --   13.93  37.00  90.00  170
 17  \w    -60.00   5.00   0.50    8.00    --   13.93 -19.00  60.00  130
 18  \w    -16.00  30.00   0.50    8.00    --   13.93  95.00 -99.00   92
 19  \w    -67.00 -19.00   0.50    8.00    --  -12.68 137.00 -76.23   96
 20  \w    -66.00 -18.00   0.50    8.00    --  -12.68 135.00  90.47   96
 21  \w    -69.00 -21.00   0.50    8.00    --  -12.68 140.00-100.23   96
 22  \w    -48.00 -14.00   0.50    8.00    --  -12.68 104.00  21.99   68
 23  \w    -66.00 -18.00   0.50    8.00    --  -12.68 135.00 149.46   96
 24  \w    -71.00 -22.00   0.50    8.00    --  -12.68 143.00 -30.19   98
 25  \w    -70.00 -22.00   0.50    8.00    --  -12.68 142.00 -56.92   96
 26  \w     23.00  75.00   0.50    8.00    --   13.93-146.00 -25.51  104
 27  \w     23.00  75.00   0.50    8.00    --   13.93-146.00 172.84  104
 28  \w    -60.00   5.00   0.50    8.00    --   13.93 -19.00 -60.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0557692000
_diffrn_orient_matrix_UB_12      -0.0408285000
_diffrn_orient_matrix_UB_13      -0.0300909000
_diffrn_orient_matrix_UB_21      0.0101616000
_diffrn_orient_matrix_UB_22      0.0587448000
_diffrn_orient_matrix_UB_23      -0.0141455000
_diffrn_orient_matrix_UB_31      0.0645776000
_diffrn_orient_matrix_UB_32      -0.0055167000
_diffrn_orient_matrix_UB_33      -0.0124312000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            115173
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.956
_diffrn_reflns_theta_min         2.433
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.010
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       plate
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.022
_refine_diff_density_max         2.482
_refine_diff_density_min         -2.241
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         13578
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+9.9957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10608
_reflns_number_total             13578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06135g2.cif
_cod_data_source_block           cx3175_auto
_cod_depositor_comments
'Adding full bibliography for 7134148--7134154.cif.'
_cod_database_code               7134154
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C29H33ClN4PPtSBF4
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.455
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F006-B01A \\sim F0-B01B
 with sigma of 0.02
 C15-C29 \\sim C15-C29A
 with sigma of 0.02
 C15-C16 \\sim C15-C16A
 with sigma of 0.02
 F008-B01A \\sim F1-B01B
 with sigma of 0.02
 F00B-B01A \\sim F00C-B01B
 with sigma of 0.02
 C29-C19 \\sim C29A-C19A
 with sigma of 0.02
 C16-C17 \\sim C16A-C17A
 with sigma of 0.02
 F00P-B01A \\sim F00Q-B01B
 with sigma of 0.02
 F006-F008 \\sim F0-F1
 with sigma of 0.04
 C19-C18 \\sim C19A-C18A
 with sigma of 0.02
 F006-F00B \\sim F0-F00C
 with sigma of 0.04
 C17-C18 \\sim C17A-C18A
 with sigma of 0.02
 F006-F00P \\sim F0-F00Q
 with sigma of 0.04
 C15-C19 \\sim C15-C19A
 with sigma of 0.04
 F008-F00B \\sim F1-F00C
 with sigma of 0.04
 C15-C17 \\sim C15-C17A
 with sigma of 0.04
 F008-F00P \\sim F1-F00Q
 with sigma of 0.04
 C29-C18 \\sim C29A-C18A
 with sigma of 0.04
 C16-C18 \\sim C16A-C18A
 with sigma of 0.04
 F00B-F00P \\sim F00C-F00Q
 with sigma of 0.04
 C19-C17 \\sim C19A-C17A
 with sigma of 0.04
 C9-C14 \\sim C9-C14A
 with sigma of 0.02
 C9-C10 \\sim C9-C10A
 with sigma of 0.02
 C14-C13 \\sim C14A-C13A
 with sigma of 0.02
 C10-C11 \\sim C10A-C11A
 with sigma of 0.02
 C13-C12 \\sim C13A-C12A
 with sigma of 0.02
 C12-C11 \\sim C12A-C11A
 with sigma of 0.02
 C9-C13 \\sim C9-C13A
 with sigma of 0.04
 C9-C11 \\sim C9-C11A
 with sigma of 0.04
 C14-C12 \\sim C14A-C12A
 with sigma of 0.04
 C10-C12 \\sim C10A-C12A
 with sigma of 0.04
 C13-C11 \\sim C13A-C11A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 F006, F008, F00B, F00P, B01A, F0, F1, F00C, F00Q, B01B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29A, C16A, C19A, C17A, C18A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C14, C10, C13, C12, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14A, C10A, C13A, C12A, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, C16, C19, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(B01B)=Sof(F0)=Sof(F1)=Sof(F00C)=Sof(F00Q)=1-FVAR(1)
 Sof(F006)=Sof(F008)=Sof(F00B)=Sof(F00P)=Sof(B01A)=FVAR(1)
 Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=
 Sof(H13A)=Sof(C14A)=Sof(H14A)=1-FVAR(2)
 Sof(C14)=Sof(H14)=Sof(C10)=Sof(H10)=Sof(C13)=Sof(H13)=Sof(C12)=Sof(H12)=
 Sof(C11)=Sof(H11)=FVAR(2)
 Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=
 Sof(H19A)=Sof(C29A)=Sof(H29A)=1-FVAR(3)
 Sof(C29)=Sof(H29)=Sof(C16)=Sof(H16)=Sof(C19)=Sof(H19)=Sof(C17)=Sof(H17)=
 Sof(C18)=Sof(H18)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C24(H24A,H24B)
5.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C29(H29), C22(H22), C14(H14), C27(H27), C16(H16), C2(H2), C26(H26),
 C3(H3), C10(H10), C19(H19), C17(H17), C13(H13), C6(H6), C12(H12), C4(H4),
 C18(H18), C11(H11), C5(H5), C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A),
 C14A(H14A), C16A(H16A), C17A(H17A), C18A(H18A), C19A(H19A), C29A(H29A)
5.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C28(H28A,H28B,H28C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              10747
_shelx_hkl_checksum              30615
_shelx_fab_checksum              21506
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.397
_oxdiff_exptl_absorpt_empirical_full_min 0.804