Coordination mode and stability of the tetrahydroborate ligand in group 10 metal pincer complexes
Chang, Jiarui; Ding, Man; Kang, Jiaxin; Zhang, Jie; Chen, Xuenian; Dalton Transactions  (2022) –; doi:10.1039/D2DT01357F

data_7710683
_publ_section_title
;
 Coordination mode and stability of the tetrahydroborate ligand in group
 10 metal pincer complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01357F
_journal_year                    2022
_chemical_formula_moiety         'C24 H48 B2 N2 P2 Pt'
_chemical_formula_sum            'C24 H48 B2 N2 P2 Pt'
_chemical_formula_weight         643.29
_chemical_name_systematic        tBu-PBP-Pt-BH4
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-29 deposited with the CCDC.	2022-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.04790(10)
_cell_length_b                   14.5349(2)
_cell_length_c                   32.1411(3)
_cell_measurement_reflns_used    15475
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      71.3190
_cell_measurement_theta_min      4.5680
_cell_volume                     5628.39(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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   -102.00 -14.00   1.00    1.00    --  -35.62 -67.00  -9.00   88
  2  \w   -103.00 -56.00   1.00    1.00    --  -35.62-151.00 120.00   47
  3  \w    -32.00  52.00   1.00    1.00    --   35.62 -54.00 153.00   84
  4  \w     41.00 128.00   1.00    1.50    --  107.12 -67.00  -9.00   87
  5  \w     40.00 124.00   1.00    1.50    --  107.12 -54.00 153.00   84
  6  \w     38.00 116.00   1.00    1.50    --  107.12-122.00 -78.00   78
  7  \w     91.00 175.00   1.00    1.50    --  107.12  54.00 -62.00   84
  8  \w   -108.00 -35.00   1.00    1.00    --  -35.62-178.00  30.00   73
  9  \w      1.00  75.00   1.00    1.00    --   35.62 -99.00   0.00   74
 10  \w     89.00 174.00   1.00    1.50    --  107.12  61.00 -90.00   85
 11  \w     38.00 110.00   1.00    1.50    --  107.12 -95.00 -30.00   72
 12  \w     37.00 113.00   1.00    1.50    --  107.12-111.00 150.00   76
 13  \w   -103.00 -19.00   1.00    1.00    --  -35.62 -57.00-120.00   84
 14  \w   -103.00 -33.00   1.00    1.00    --  -35.62 -57.00  60.00   70
 15  \w   -103.00  -9.00   1.00    1.00    --  -35.62 -77.00 150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0579077000
_diffrn_orient_matrix_UB_12      -0.0438921000
_diffrn_orient_matrix_UB_13      -0.0378541000
_diffrn_orient_matrix_UB_21      -0.0592140000
_diffrn_orient_matrix_UB_22      -0.0686776000
_diffrn_orient_matrix_UB_23      0.0290086000
_diffrn_orient_matrix_UB_31      -0.0973695000
_diffrn_orient_matrix_UB_32      0.0677839000
_diffrn_orient_matrix_UB_33      0.0048609000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            27062
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.536
_diffrn_reflns_theta_min         4.587
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.487
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.077
_refine_diff_density_min         -1.235
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5401
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+20.7432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4980
_reflns_number_total             5401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01357f2.cif
_cod_data_source_block           pbp-pt-bh4-dyz
_cod_database_code               7710683
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 B1 P1 N1 Pt1 '
_shelx_estimated_absorpt_t_max   0.392
_shelx_estimated_absorpt_t_min   0.285
_diffrn_oxdiff_digest_frames
;
01d7b2913f1dfcbdf855908f0b4a577da3000324485
;
_diffrn_oxdiff_digest_hkl
;
0145a30865362171ba55bb768a6cf51f05e5e5
;
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C4(H4), C5(H5), C6(H6)
3.c Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C15(H15a,H15b,
 H15c), C14(H14a,H14b,H14c), C16(H16a,H16b,H16c), C18(H18a,H18b,H18c), C22(H22a,
 H22b,H22c), C20(H20a,H20b,H20c), C24(H24b,H24c,H24a), C19(H19a,H19b,H19c),
 C23(H23b,H23a,H23c)
;
_shelx_res_checksum              17412
_shelx_hkl_checksum              29686
_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 2.279
_oxdiff_exptl_absorpt_empirical_full_min 0.561