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_7134149
_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 N4 P Pt S, 2(B F4)'
_chemical_formula_sum            'C29 H31 B2 F8 N4 P Pt S'
_chemical_formula_weight         867.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 94.137(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1155(2)
_cell_length_b                   20.5747(4)
_cell_length_c                   15.5888(3)
_cell_measurement_reflns_used    21563
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      31.2560
_cell_measurement_theta_min      2.3790
_cell_volume                     3235.94(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (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      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.804
_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    -76.00  67.00   0.50    3.72    --   -4.61   0.00 -90.00  286
  2  \w    -23.00  28.00   0.50    3.72    --   -4.61 -99.00 120.00  102
  3  \w    -19.00  68.00   0.50    3.72    --   -4.61  57.00  30.00  174
  4  \w    -20.00  25.00   0.50    3.72    --   -4.61 -99.00 -90.00   90
;
_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      0.0473600000
_diffrn_orient_matrix_UB_12      0.0216038000
_diffrn_orient_matrix_UB_13      -0.0156101000
_diffrn_orient_matrix_UB_21      -0.0338721000
_diffrn_orient_matrix_UB_22      0.0267000000
_diffrn_orient_matrix_UB_23      0.0170555000
_diffrn_orient_matrix_UB_31      0.0394020000
_diffrn_orient_matrix_UB_32      -0.0029846000
_diffrn_orient_matrix_UB_33      0.0393254000
_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  0.0378
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.804
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37346
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.804
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.060
_diffrn_reflns_theta_min         1.980
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.524
_exptl_absorpt_correction_T_max  0.07215
_exptl_absorpt_correction_T_min  0.04372
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       sphere
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.067
_exptl_crystal_size_rad          0.086
_refine_diff_density_max         3.864
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         8342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+3.9387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6889
_reflns_number_total             8342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06135g2.cif
_cod_data_source_block           fw-351-1_auto
_cod_depositor_comments
'Adding full bibliography for 7134148--7134154.cif.'
_cod_database_code               7134149
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C Pt N B F P S'
_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.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C23(H23A,H23B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C7(H7), C11(H11), C29(H29), C8(H8), C17(H17), C13(H13),
 C12(H12), C20(H20), C25(H25), C21(H21), C28(H28), C14(H14), C27(H27), C15(H15),
  C19(H19), C26(H26), C18(H18)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              35256
_shelx_hkl_checksum              22104
_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 1.650
_oxdiff_exptl_absorpt_empirical_full_min 0.759