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_7712306
_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, 1.5[C3H6O]'
_chemical_formula_sum            'C34.5 H51 B11 N3 O1.5 Pt'
_chemical_formula_weight         845.78
_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             2023-02-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-03 deposited with the CCDC.	2023-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.6890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.42200(10)
_cell_length_b                   16.90720(10)
_cell_length_c                   31.1951(2)
_cell_measurement_reflns_used    23258
_cell_measurement_temperature    295.58(10)
_cell_measurement_theta_max      77.0520
_cell_measurement_theta_min      2.6130
_cell_volume                     3910.21(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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_environment      air
_diffrn_ambient_temperature      295.58(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     92.00 148.00   0.50    1.51    --  108.56  61.00 120.00  112
  2  \w    153.00 178.00   0.50    1.51    --  108.56  61.00 120.00   50
  3  \w    107.00 175.00   0.50    1.51    --  108.56  45.00  30.00  136
  4  \w    141.00 167.00   0.50    1.51    --  108.56  15.00-150.00   52
  5  \w     95.00 130.00   0.50    1.51    --  108.56  15.00-150.00   70
  6  \w     58.00 102.00   0.50    1.51    --  108.56 -94.00 -90.00   88
  7  \w     37.00 104.00   0.50    1.51    --  108.56 -94.00 -30.00  134
  8  \w     10.00  51.00   0.50    0.50    --   47.12-101.00 158.00   82
  9  \w     48.00 105.00   0.50    1.51    --  108.56-101.00 158.00  114
 10  \w     -1.00  24.00   0.50    0.50    --   47.12 -19.00-120.00   50
 11  \w     42.00  69.00   0.50    1.51    --  108.56 -61.00-150.00   54
 12  \w     36.00  71.00   0.50    1.51    --  108.56 -61.00   0.00   70
 13  \w     43.00  71.00   0.50    1.51    --  108.56 -61.00  30.00   56
 14  \w     39.00  71.00   0.50    1.51    --  108.56 -61.00  60.00   64
 15  \w     36.00  81.00   0.50    1.51    --  108.56 -77.00 150.00   90
 16  \w     39.00  71.00   0.50    1.51    --  108.56 -61.00 -30.00   64
 17  \w     39.00  65.00   0.50    1.51    --  108.56 -61.00 -60.00   52
 18  \w     36.00  71.00   0.50    1.51    --  108.56 -61.00-120.00   70
 19  \w    126.00 153.00   0.50    1.51    --  108.56 101.00 -96.00   54
 20  \w    -50.00 -23.00   0.50    1.51    --  -88.50  45.00 -90.00   54
 21  \w    -47.00 -16.00   0.50    1.51    --  -88.50  45.00-150.00   62
 22  \w    -80.00  15.00   0.50    0.50    --  -47.12 101.00 -96.00  190
 23  \w    -53.00 -27.00   0.50    1.51    --  -88.50 101.00 -96.00   52
 24  \w    -51.00 -17.00   0.50    1.51    --  -88.50  45.00 120.00   68
 25  \w   -110.00 -73.00   0.50    0.50    --  -47.12-125.00 -30.00   74
 26  \w   -153.00-117.00   0.50    1.51    --  -88.50 -61.00-180.00   72
 27  \w    -97.00 -72.00   0.50    1.51    --  -88.50 -61.00-180.00   50
 28  \w   -113.00 -79.00   0.50    0.50    --  -47.12-125.00-150.00   68
 29  \w   -115.00 -81.00   0.50    0.50    --  -47.12-125.00-120.00   68
 30  \w   -117.00 -91.00   0.50    1.51    --  -88.50-101.00 158.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0725412000
_diffrn_orient_matrix_UB_12      0.0453120000
_diffrn_orient_matrix_UB_13      0.0400189000
_diffrn_orient_matrix_UB_21      -0.1654676000
_diffrn_orient_matrix_UB_22      -0.0263813000
_diffrn_orient_matrix_UB_23      0.0243961000
_diffrn_orient_matrix_UB_31      0.1027299000
_diffrn_orient_matrix_UB_32      -0.0745107000
_diffrn_orient_matrix_UB_33      0.0157209000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            29150
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.262
_diffrn_reflns_theta_min         2.974
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.953
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42973
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_refine_diff_density_max         1.026
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7951
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+3.7333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7697
_reflns_number_total             7951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00136a2.cif
_cod_data_source_block           20210925-hfp-bhd-kxj-45
_cod_original_formula_sum        'C34.50 H51 B11 N3 O1.50 Pt'
_cod_database_code               7712306
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C116 H112 B44 N20 Pt4 O1 '
_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. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C30(H30), C8(H8), C23(H23), C11(H11), C4(H4), C29(H29),
 C20(H20), C3(H3), C5(H5), C9(H9), C2(H2)
3.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C)
3.c Boron cage BH refined with riding coordinates:
 B3(H3A), B2(H2A), B5(H5A), B1(H1), B11(H11A), B8(H8A), B4(H4A), B7(H7),
 B9(H9A), B6(H6), B10(H10)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 192 electrons were 
found in a volume of 956\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[C3H6O] per Asymmetric Unit 
which account for 192 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              74848
_shelx_fab_checksum              87791
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.996
_oxdiff_exptl_absorpt_empirical_full_min 0.520