Platinum(II) Diimine Complexes Containing Phenylpyridine Ligands Decorated with Anionic closo-Monocarborane Clusters [CB11H12]-
Kong, Xiangjun; Shen, Yunjun; Bian, He-Dong; Zhang, Yuzhen; Dalton Transactions  (2023) –; doi:10.1039/D3DT00136A

data_7712305
_publ_section_title
;
 Platinum(II) Diimine Complexes Containing Phenylpyridine Ligands
 Decorated with Anionic closo-Monocarborane Clusters [CB11H12]-
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00136A
_journal_year                    2023
_chemical_formula_moiety         'C30 H42 B11 N3 Pt, 1[CH3COCH3]'
_chemical_formula_sum            'C33 H48 B11 N3 O Pt'
_chemical_formula_weight         816.74
_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             2023-02-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-01 deposited with the CCDC.	2023-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.726(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8313(2)
_cell_length_b                   21.0697(7)
_cell_length_c                   22.2923(7)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    213.15
_cell_measurement_theta_max      54.958
_cell_measurement_theta_min      3.474
_cell_volume                     3652.98(19)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      213.15
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26299
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.057
_diffrn_reflns_theta_min         3.474
_diffrn_source_current           2.86
_diffrn_source_power             0.1995994
_diffrn_source_voltage           69.79
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.084
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1317 before and 0.0894 after correction.
The Ratio of minimum to maximum transmission is 0.7002.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.436
_refine_diff_density_min         -2.791
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6824
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0780
_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^)+(0.1306P)^2^+7.7236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2313
_refine_ls_wR_factor_ref         0.2516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4986
_reflns_number_total             6824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00136a2.cif
_cod_data_source_block           210916kxj_0m_pl
_cod_database_code               7712305
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H12-H22
 2.1 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C27 \\sim C28 \\sim C29 \\sim C30: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C19(H19), C21(H21), C22(H22)
4.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
4.c Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3A), B4(H4A), B5(H5), B6(H6), B7(H7A), B8(H8), B9(H9A),
 B10(H10A), B11(H11A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 62 electrons were 
found in a volume of 568\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH3COCH3] per Formula Unit 
which account for 128 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              54608
_shelx_fab_checksum              64890
_olex2_submission_special_instructions 'No special instructions were received'