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_7712307
_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         'C42 H50 B11 N3 Pt, 0.5(C3 H6 O)'
_chemical_formula_sum            'C43.5 H53 B11 N3 O0.5 Pt'
_chemical_formula_weight         968.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/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                 100.113(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   14.7529(7)
_cell_length_b                   34.2378(15)
_cell_length_c                   40.5905(19)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    213.00
_cell_measurement_theta_max      53.961
_cell_measurement_theta_min      2.443
_cell_volume                     20184.0(16)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      213.00
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.982
_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  0.1599
_diffrn_reflns_av_unetI/netI     0.1662
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            94522
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.193
_diffrn_reflns_theta_min         2.443
_diffrn_source_current           2.86
_diffrn_source_power             0.1995708
_diffrn_source_voltage           69.78
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.736
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1518 before and 0.0894 after correction.
The Ratio of minimum to maximum transmission is 0.6617.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             7808
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.735
_refine_diff_density_min         -1.720
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1051
_refine_ls_number_reflns         19042
_refine_ls_number_restraints     497
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.2179
_refine_ls_R_factor_gt           0.1160
_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^)+(0.1761P)^2^+32.9237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2835
_refine_ls_wR_factor_ref         0.3436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8253
_reflns_number_total             19042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00136a2.cif
_cod_data_source_block           220110kxj_0m
_cod_depositor_comments
;

2024-09-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C90 H112 B22 N6 O2 Pt2'
_cod_original_formula_weight         1937.85
_cod_original_formula_moiety    '2(C42 H50 B11 N3 Pt), C3 H6 O, 1[CH3COCH3]'
_cod_original_formula_units_Z            8
_cod_database_code               7712307
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.896
_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
 C81-C78
 1.53 with sigma of 0.01
 C81-C82 = C81-C84
 1.53 with sigma of 0.01
 C29-C26 = C32-C29 = C31-C29 = C30-C29
 1.53 with sigma of 0.01
 C81-C83
 1.53 with sigma of 0.01
 C30-C32
 2.44 with sigma of 0.01
 C30-C31
 2.44 with sigma of 0.01
 H37-H42A = H31C-H84B_$1 = H25-H30A
 2.1 with sigma of 0.01
 H79-H82A
 2.1 with sigma of 0.01
 C84-C82 \\sim C82-C83
 with sigma of 0.02
3. Rigid bond restraints
 B9, B11, B4, B9, N1, C11
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C39, C40, B6, B7
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 B9, B10
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 B8, B9
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C78 \\sim C77 \\sim C76 \\sim C75 \\sim C81 \\sim C82 \\sim C83 \\sim C84:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C29 \\sim C30 \\sim C31 \\sim C32: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C54 \\sim B12 \\sim B13 \\sim B14 \\sim B15 \\sim B16 \\sim B17 \\sim B18 \\sim
B19 \\sim B20 \\sim B21 \\sim B22: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C20 \\sim C23 \\sim C24 \\sim C28: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N6 \\sim C63 \\sim C64: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N2 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
5.a Me refined with riding coordinates:
 C32(H32A,H32B,H32C), C84(H84A,H84B,H84C)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C13(H13), C14(H14),
 C16(H16), C19(H19), C21(H21), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28),
  C34(H34), C35(H35), C37(H37), C38(H38), C44(H44), C45(H45), C46(H46),
 C47(H47), C50(H50), C51(H51), C53(H53), C55(H55), C56(H56), C58(H58), C61(H61),
  C63(H63), C64(H64), C66(H66), C67(H67), C69(H69), C70(H70), C80(H80),
 C79(H79), C77(H77), C76(H76)
5.c Fitted hexagon refined as free rotating group:
 C43(C44,C45,C46,C47,C48), C80(C79,C78,C77,C76,C75)
5.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,
 H74B,H74C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C86(H86A,H86B,H86C),
 C87(H87A,H87B,H87C)
5.e Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2A), B3(H3A), B4(H4A), B5(H5A), B6(H6), B7(H7), B8(H8A), B9(H9A),
 B10(H10), B11(H11A), B12(H12), B13(H13A), B14(H14A), B15(H15), B16(H16A),
 B17(H17), B18(H18), B19(H19A), B20(H20), B21(H21A), B22(H22A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 589 electrons were 
found in a volume of 4859\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[CH3COCH3] per Formula Unit 
which account for 256 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              66839
_shelx_fab_checksum              39174
_olex2_submission_special_instructions 'No special instructions were received'