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_7134219
_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         'C66 H97 B2 Br2 N2 P3 Pt2'
_chemical_formula_sum            'C66 H97 B2 Br2 N2 P3 Pt2'
_chemical_formula_weight         1582.98
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-12
_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                 112.643(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.9051(7)
_cell_length_b                   13.8819(4)
_cell_length_c                   19.7934(9)
_cell_measurement_reflns_used    20281
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.84
_cell_measurement_theta_min      2.23
_cell_volume                     4033.4(3)
_computing_cell_refinement
;
X-Area Recipe 2.0.1 (STOE, 2023)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.192.0 (STOE, 2023)
;
_computing_data_reduction
;
X-Area Integrate 2.5.15.0 (STOE, 2023)
X-Area LANA 2.7.12 (STOE, 2023)
;
_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      100.0
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
 439 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.1097
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24339
_diffrn_reflns_point_group_measured_fraction_full 0.799
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.230
_exptl_absorpt_coefficient_mu    4.547
_exptl_absorpt_correction_T_max  0.9257
_exptl_absorpt_correction_T_min  0.7245
_exptl_absorpt_correction_type   multi-scan
_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. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.071
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.990
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.216
_refine_ls_abs_structure_details
;
 Flack x determined using 2678 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.034(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         12599
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0947P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.592
_reflns_Friedel_fraction_full    0.602
_reflns_Friedel_fraction_max     0.592
_reflns_number_gt                9546
_reflns_number_total             12599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06268j2.cif
_cod_data_source_block           2d
_cod_depositor_comments
'Adding full bibliography for 7134213--7134220.cif.'
_cod_database_code               7134219
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 P1-C25 \\sim P1-C25A
 with sigma of 0.02
 C25-C26 \\sim C25A-C26A \\sim C25-C30 \\sim C25A-C30A
 with sigma of 0.02
 C26-C27 \\sim C26A-C27A \\sim C27-C28 \\sim C27A-C28A
 with sigma of 0.02
 C28-C29 \\sim C28A-C29A \\sim C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 P1-C26 \\sim P1-C26A
 with sigma of 0.04
 P1-C30 \\sim P1-C30A
 with sigma of 0.04
 C25-C27 \\sim C25A-C27A
 with sigma of 0.04
 C25-C29 \\sim C25A-C29A
 with sigma of 0.04
 C26-C28 \\sim C26A-C28A
 with sigma of 0.04
 C26-C30 \\sim C26A-C30A
 with sigma of 0.04
 C27-C29 \\sim C27A-C29A
 with sigma of 0.04
 C28-C30 \\sim C28A-C30A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
N2 \\sim B2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C35 \\sim C36: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C56 \\sim C57: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C25(0.5) C26(0.5) H26(0.5) C27(0.5) H27(0.5) C28(0.5) H28(0.5)
 C29(0.5) H29(0.5) C30(0.5) H30(0.5) C25A(0.5) C26A(0.5) H26A(0.5) C27A(0.5)
 H27A(0.5) C28A(0.5) H28A(0.5) C29A(0.5) H29A(0.5) C30A(0.5) H30A(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7), C13(H13), C19(H19), C49(H49), C55(H55), C61(H61)
5.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),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C50(H50A,
 H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B),
 C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B),
  C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B)
5.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C26A(H26A), C27A(H27A),
 C28A(H28A), C29A(H29A), C30A(H30A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37036
_shelx_hkl_checksum              23943
_olex2_submission_special_instructions 'No special instructions were received'