Side-on phosphinoboryl platinum(II) complexes.
Ordyszewska, Anna; Czaplewski, Antoni; Wojnowski, Tomasz; Anusiewicz, Iwona; Chojnacki, Jarosław; Grubba, Rafał; Chemical communications (Cambridge, England) 61 (2025) 3728–3731; doi:10.1039/d4cc06268j

data_7134213
_publ_section_title
;
 Side-on phosphinoboryl platinum(II) complexes.
;
_journal_issue                   18
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3728
_journal_page_last               3731
_journal_paper_doi               10.1039/d4cc06268j
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         '2(C32 H47 B Br N P2 Pt), 2(C7 H8), C H2 Cl2'
_chemical_formula_sum            'C79 H112 B2 Br2 Cl2 N2 P4 Pt2'
_chemical_formula_weight         1856.10
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-11-12 deposited with the CCDC.	2025-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                74.577(9)
_cell_angle_beta                 85.390(9)
_cell_angle_gamma                82.420(9)
_cell_formula_units_Z            1
_cell_length_a                   11.0758(11)
_cell_length_b                   11.5452(14)
_cell_length_c                   17.0605(19)
_cell_measurement_reflns_used    57186
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      67.45
_cell_measurement_theta_min      2.69
_cell_volume                     2082.3(4)
_computing_cell_refinement       'X-Area Recipe 1.34.0.0 (STOE, 2019)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_computing_data_reduction
'X-Area Integrate 1.77.0.0 (STOE, 2019) X-Area X-Red32 1.65.0.0 (STOE, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17035
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        62.489
_diffrn_reflns_theta_max         62.489
_diffrn_reflns_theta_min         2.690
_diffrn_source                   'GeniX Cu, 0.05 x 0.05 mm2 microfocus'
_exptl_absorpt_coefficient_mu    8.933
_exptl_absorpt_correction_T_max  0.7272
_exptl_absorpt_correction_T_min  0.1353
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'STOE X-Red32, absorption correction by Gaussian integration, analogous to P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis", published in F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard, Copenhagen (1970), 255 - 270'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.035
_refine_diff_density_max         2.681
_refine_diff_density_min         -3.216
_refine_diff_density_rms         0.279
_refine_ls_extinction_coef       0.0039(4)
_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   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         6413
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0932
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1763P)^2^+25.6281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2426
_refine_ls_wR_factor_ref         0.2593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5540
_reflns_number_total             6413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06268j2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7134213--7134220.cif.'
_cod_database_code               7134213
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.745
_shelx_estimated_absorpt_t_min   0.173
_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
 C40-Cl1 \\sim C40-Cl2 \\sim C40A-Cl3 \\sim C40A-Cl4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim Cl3 \\sim Cl4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C40 \\sim C40A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
4. Others
 Sof(Cl3)=Sof(Cl4)=Sof(C40A)=Sof(H40C)=Sof(H40D)=0.5*(1-FVAR(2))
 Sof(Cl1)=Sof(Cl2)=Sof(C40)=Sof(H40A)=Sof(H40B)=0.5*FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
5.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C40A(H40C,H40D)
5.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
  C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
5.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              87931
_shelx_hkl_checksum              43949
_olex2_submission_special_instructions 'No special instructions were received'