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_7134148
_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 H32 N5 P Pt S, 2(B F4)'
_chemical_formula_sum            'C30 H32 B2 F8 N5 P Pt S'
_chemical_formula_weight         894.34
_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
_audit_creation_date             2023-08-30
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-09-18 deposited with the CCDC.	2025-01-01 downloaded from the CCDC.
;
_cell_angle_alpha                101.9598(10)
_cell_angle_beta                 103.3600(10)
_cell_angle_gamma                103.1011(10)
_cell_formula_units_Z            2
_cell_length_a                   11.57903(12)
_cell_length_b                   11.85721(14)
_cell_length_c                   13.18425(17)
_cell_measurement_reflns_used    59384
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      34.0040
_cell_measurement_theta_min      2.7260
_cell_volume                     1649.68(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.918
_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    -67.00 -20.00   0.50   15.00    --  -12.68 138.00-169.00   94
  2  \w    -62.00 -16.00   0.50   15.00    --  -12.68 131.00  15.00   92
  3  \w     20.00  69.00   0.50   15.00    --   13.93-138.00 128.00   98
  4  \w     16.00  64.00   0.50   15.00    --   13.93-131.00 -55.00   96
  5  \w    -40.00  43.00   0.50   15.00    --  -12.68  87.00  93.65  166
  6  \w    -24.00  21.00   0.50   15.00    --  -12.68 -99.00 120.00   90
  7  \w    -85.00  10.00   0.50   15.00    --  -12.68 -77.00  60.00  190
  8  \w    -67.00 -19.00   0.50   15.00    --  -12.68 137.00 -87.99   96
  9  \w    -85.00  10.00   0.50   15.00    --  -12.68 -77.00-120.00  190
 10  \w    -86.00   0.00   0.50   15.00    --  -12.68 -37.00-120.00  172
 11  \w    -24.00  21.00   0.50   15.00    --  -12.68 -99.00 -60.00   90
 12  \w    -34.00  45.00   0.50   15.00    --   13.93 -94.00  52.71  158
 13  \w    -42.00  42.00   0.50   15.00    --   13.93 -88.00-125.42  168
 14  \w      2.00  87.00   0.50   15.00    --   13.93  37.00 150.00  170
 15  \w    -60.00   5.00   0.50   15.00    --   13.93 -19.00 -30.00  130
 16  \w    -42.00  43.00   0.50   15.00    --   13.93 -90.00 -52.47  170
 17  \w    -60.00   5.00   0.50   15.00    --   13.93 -19.00 150.00  130
 18  \w    -24.00  21.00   0.50   15.00    --  -12.68 -99.00 -90.00   90
 19  \w    -66.00 -18.00   0.50   15.00    --  -12.68 135.00 145.70   96
 20  \w    -69.00 -21.00   0.50   15.00    --  -12.68 140.00-115.44   96
 21  \w    -69.00 -21.00   0.50   15.00    --  -12.68 140.00  33.32   96
 22  \w    -66.00 -19.00   0.50   15.00    --  -12.68 136.00 118.71   94
 23  \w    -24.00  21.00   0.50   15.00    --  -12.68 -99.00   0.00   90
 24  \w    -69.00 -21.00   0.50   15.00    --  -12.68 140.00 -14.78   96
 25  \w    -67.00 -19.00   0.50   15.00    --  -12.68 137.00 107.32   96
 26  \w    -24.00  21.00   0.50   15.00    --  -12.68 -99.00-180.00   90
 27  \w    -66.00 -18.00   0.50   15.00    --  -12.68 135.00-169.75   96
 28  \w    -60.00 -35.00   0.50   15.00    --   13.93 -19.00  30.00   50
 29  \w    -31.00  45.00   0.50   15.00    --   13.93 -95.00  30.36  152
;
_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      0.0031209000
_diffrn_orient_matrix_UB_12      -0.0073508000
_diffrn_orient_matrix_UB_13      -0.0539858000
_diffrn_orient_matrix_UB_21      0.0633566000
_diffrn_orient_matrix_UB_22      0.0341059000
_diffrn_orient_matrix_UB_23      0.0197434000
_diffrn_orient_matrix_UB_31      0.0173228000
_diffrn_orient_matrix_UB_32      -0.0534892000
_diffrn_orient_matrix_UB_33      0.0012025000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            106307
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.897
_diffrn_reflns_theta_min         2.738
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.441
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.447
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.75a (Rigaku Oxford Diffraction, 2022)
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    1.800
_exptl_crystal_description       plate
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.015
_refine_diff_density_max         5.392
_refine_diff_density_min         -1.455
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         106307
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+5.9944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                90989
_reflns_number_total             106307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06135g2.cif
_cod_data_source_block           cx3190_auto
_cod_depositor_comments
'Adding full bibliography for 7134148--7134154.cif.'
_cod_database_code               7134148
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C28H31ClN4PPtS
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.903(4)
 0.097(4)
2. 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
3. Restrained distances
 C16-C21 \\sim C16-C21A
 with sigma of 0.02
 C16-C17 \\sim C16-C17A
 with sigma of 0.02
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 C19-C18 \\sim C19A-C18A
 with sigma of 0.02
 C21-C20 \\sim C21A-C20A
 with sigma of 0.02
 C17-C18 \\sim C17A-C18A
 with sigma of 0.02
 C16-C20 \\sim C16-C20A
 with sigma of 0.04
 C16-C18 \\sim C16-C18A
 with sigma of 0.04
 C19-C21 \\sim C19A-C21A
 with sigma of 0.04
 C19-C17 \\sim C19A-C17A
 with sigma of 0.04
 C20-C18 \\sim C20A-C18A
 with sigma of 0.04
4. Rigid body (RIGU) restrains
 C19, C21, C17, C20, C18, C19A, C21A, C17A, C20A, C18A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=
 Sof(H20A)=Sof(C21A)=Sof(H21A)=1-FVAR(1)
 Sof(C19)=Sof(H19)=Sof(C21)=Sof(H21)=Sof(C17)=Sof(H17)=Sof(C20)=Sof(H20)=
 Sof(C18)=Sof(H18)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C22(H22A,H22B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C15(H15), C3(H3), C14(H14), C8(H8), C13(H13), C7(H7), C11(H11),
 C19(H19), C12(H12), C21(H21), C28(H28), C24(H24), C27(H27), C17(H17), C20(H20),
  C25(H25), C18(H18), C26(H26), C17A(H17A), C18A(H18A), C19A(H19A), C20A(H20A),
 C21A(H21A)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              33890
_shelx_hkl_checksum              258
_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 1.203
_oxdiff_exptl_absorpt_empirical_full_min 0.803