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_7134150
_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         'C30 H33 N4 P Pt S, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C32 H36 B2 F8 N5 P Pt S'
_chemical_formula_weight         922.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-08-25
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6049(6)
_cell_length_b                   19.1262(6)
_cell_length_c                   8.8690(3)
_cell_measurement_reflns_used    19097
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.5500
_cell_measurement_theta_min      2.1140
_cell_volume                     3495.21(19)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_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 0.881
_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    -81.00   6.00   0.50    9.50    --   -8.26 -56.00 -45.00  174
  2  \w    -81.00   9.00   0.50    9.50    --   -8.26 -64.00 128.00  180
  3  \w    -23.00  24.00   0.50    9.50    --   -8.26 -99.00   0.00   94
  4  \w    -23.00  42.00   0.50    9.50    --    9.51 -99.00 -90.00  130
  5  \w    -23.00  42.00   0.50    9.50    --    9.51 -99.00 -60.00  130
  6  \w    -21.00   4.00   0.50    9.50    --   -8.26  37.00  90.00   50
;
_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      -0.0209765000
_diffrn_orient_matrix_UB_12      0.0263209000
_diffrn_orient_matrix_UB_13      -0.0284755000
_diffrn_orient_matrix_UB_21      -0.0098889000
_diffrn_orient_matrix_UB_22      0.0081135000
_diffrn_orient_matrix_UB_23      0.0745725000
_diffrn_orient_matrix_UB_31      0.0254217000
_diffrn_orient_matrix_UB_32      0.0248114000
_diffrn_orient_matrix_UB_33      0.0058487000
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            45647
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.771
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.309
_diffrn_reflns_theta_min         2.130
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.195
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.314
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (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    1.753
_exptl_crystal_description       needle
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.033
_refine_diff_density_max         2.825
_refine_diff_density_min         -1.823
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Flack x determined using 2829 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(5)
_refine_ls_extinction_coef       0.00025(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         9617
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+6.3544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.658
_reflns_Friedel_fraction_full    0.881
_reflns_Friedel_fraction_max     0.649
_reflns_number_gt                7803
_reflns_number_total             9617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06135g2.cif
_cod_data_source_block           cx3078_auto
_cod_depositor_comments
'Adding full bibliography for 7134148--7134154.cif.'
_cod_original_cell_volume        3495.22(19)
_cod_database_code               7134150
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30N4PPtS
_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:
 C23(H23A,H23B), C11(H11A,H11B), C22(H22A,H22B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C16(H16), C20(H20), C2(H2), C1(H1), C28(H28), C12(H12), C32(H32),
 C18(H18), C13(H13), C9(H9), C6(H6), C31(H31), C19(H19), C5(H5), C17(H17),
 C30(H30), C29(H29), C8(H8)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C7(H7A,H7B,H7C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              2599
_shelx_hkl_checksum              49544
_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 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.757