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_7134220
_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         'C36 H69 B Br N P2 Pt'
_chemical_formula_sum            'C36 H69 B Br N P2 Pt'
_chemical_formula_weight         863.67
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2024-11-07
_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                90
_cell_angle_beta                 101.65(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.351(3)
_cell_length_b                   16.632(3)
_cell_length_c                   19.686(5)
_cell_measurement_reflns_used    2640
_cell_measurement_temperature    220
_cell_measurement_theta_max      50.21
_cell_measurement_theta_min      3.41
_cell_volume                     3960.6(16)
_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      220.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0410
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24127
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        66.769
_diffrn_reflns_theta_max         66.769
_diffrn_reflns_theta_min         3.510
_diffrn_source                   'GeniX Cu, 0.05 x 0.05 mm2 microfocus'
_exptl_absorpt_coefficient_mu    8.732
_exptl_absorpt_correction_T_max  0.7284
_exptl_absorpt_correction_T_min  0.3224
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.885
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6783
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0490
_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^)+50.2536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4898
_reflns_number_total             6783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06268j2.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 7134213--7134220.cif.'
_cod_original_cell_volume        3960.4(16)
_cod_database_code               7134220
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.780
_shelx_estimated_absorpt_t_min   0.354
_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
 P1-C7 \\sim P1-C7A
 with sigma of 0.02
 C7-C8 \\sim C7A-C12A
 with sigma of 0.02
 C7-C12 \\sim C7A-C8A
 with sigma of 0.02
 C8-C9 \\sim C12A-C11A
 with sigma of 0.02
 C9-C10 \\sim C11A-C10A
 with sigma of 0.02
 C11-C12 \\sim C9A-C8A
 with sigma of 0.02
 C11-C10 \\sim C9A-C10A
 with sigma of 0.02
 P1-C8 \\sim P1-C12A
 with sigma of 0.04
 P1-C12 \\sim P1-C8A
 with sigma of 0.04
 C7-C9 \\sim C7A-C11A
 with sigma of 0.04
 C7-C11 \\sim C7A-C9A
 with sigma of 0.04
 C8-C12 \\sim C12A-C8A
 with sigma of 0.04
 C8-C10 \\sim C12A-C10A
 with sigma of 0.04
 C9-C11 \\sim C11A-C9A
 with sigma of 0.04
 C12-C10 \\sim C8A-C10A
 with sigma of 0.04
3. Others
 Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=
 Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7), C7A(H7A), C13(H13), C16(H16), C19(H19), C25(H25), C31(H31)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B),
 C8A(H8AA,H8AB), C9(H9A,H9B), C9A(H9AA,H9AB), C10(H10A,H10B), C10A(H10C,H10D),
 C11(H11A,H11B), C11A(H11C,H11D), C12(H12A,H12B), C12A(H12C,H12D), C20(H20A,
 H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              73681
_shelx_hkl_checksum              59993
_olex2_submission_special_instructions 'No special instructions were received'