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_7134152
_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         'C33 H38 N5 P Pt S, 2(B F4)'
_chemical_formula_sum            'C33 H38 B2 F8 N5 P Pt S'
_chemical_formula_weight         936.42
_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                68.424(2)
_cell_angle_beta                 79.210(2)
_cell_angle_gamma                73.111(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3866(2)
_cell_length_b                   12.6158(2)
_cell_length_c                   15.7425(3)
_cell_measurement_reflns_used    32719
_cell_measurement_temperature    113(19)
_cell_measurement_theta_max      31.2970
_cell_measurement_theta_min      2.3700
_cell_volume                     1828.04(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (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      113(19)
_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 0.822
_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    -70.00   5.00   0.50    1.00    --    5.70 -19.00 150.00  150
  2  \w    -67.00  21.00   0.50    1.00    --    5.70 -57.00  30.00  176
  3  \w    -70.00   5.00   0.50    1.00    --    5.70 -19.00 -90.00  150
  4  \w    -23.00  38.00   0.50    1.00    --    5.70 -99.00-150.00  122
  5  \w    -23.00  28.00   0.50    1.00    --   -4.45 -99.00 -90.00  102
  6  \w    -80.00   5.00   0.50    1.00    --   -4.45 -19.00-150.00  170
  7  \w    -23.00  28.00   0.50    1.00    --   -4.45 -99.00  30.00  102
  8  \w    -77.00  11.00   0.50    1.00    --   -4.45 -57.00  90.00  176
  9  \w    -23.00  28.00   0.50    1.00    --   -4.45 -99.00 150.00  102
;
_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      0.0299706000
_diffrn_orient_matrix_UB_12      -0.0253775000
_diffrn_orient_matrix_UB_13      -0.0346081000
_diffrn_orient_matrix_UB_21      -0.0150987000
_diffrn_orient_matrix_UB_22      0.0563097000
_diffrn_orient_matrix_UB_23      -0.0340337000
_diffrn_orient_matrix_UB_31      0.0633176000
_diffrn_orient_matrix_UB_32      0.0083233000
_diffrn_orient_matrix_UB_33      0.0032920000
_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  0.0979
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40669
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.913
_diffrn_reflns_theta_min         2.327
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.012
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
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    1.701
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.585
_refine_diff_density_min         -3.985
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         9492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0659P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8720
_reflns_number_total             9492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06135g2.cif
_cod_data_source_block           fw-353-1_auto
_cod_depositor_comments
'Adding full bibliography for 7134148--7134154.cif.'
_cod_original_cell_volume        1828.04(7)
_cod_database_code               7134152
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C Pt N B F P S'
_shelx_estimated_absorpt_t_max   0.584
_shelx_estimated_absorpt_t_min   0.234
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H9A,H9B,H9C} of C9, All C(H,H) groups
 At 1.5 times of:
  {H1A,H1B,H1C} of C1, {H33A,H33B,H33C} of C33
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C24(H24A,H24B), C5(H5A,H5B), C23(H23A,H23B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C15(H15), C4(H4), C21(H21), C17(H17), C19(H19), C11(H11),
 C7(H7), C14(H14), C20(H20), C12(H12), C18(H18), C13(H13), C27(H27), C28(H28),
 C31(H31), C29(H29), C30(H30)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C33(H33A,H33B,H33C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              74065
_shelx_hkl_checksum              26885
_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 1.646
_oxdiff_exptl_absorpt_empirical_full_min 0.624