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_7710682
_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         'C22 H43 B O2 P2 Pt'
_chemical_formula_sum            'C22 H43 B O2 P2 Pt'
_chemical_formula_weight         607.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 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                100.600(5)
_cell_angle_beta                 95.298(5)
_cell_angle_gamma                105.175(5)
_cell_formula_units_Z            2
_cell_length_a                   8.3424(4)
_cell_length_b                   12.3156(8)
_cell_length_c                   13.4994(9)
_cell_measurement_reflns_used    2511
_cell_measurement_temperature    295.56(10)
_cell_measurement_theta_max      21.8700
_cell_measurement_theta_min      4.0790
_cell_volume                     1301.24(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.56(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0528
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.872
_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    -20.00  55.00   1.00    1.00    --   15.98 -99.00 150.00   75
  2  \w    -11.00  84.00   1.00    1.00    --   15.98  77.00 -30.00   95
  3  \w     -1.00  83.00   1.00    1.00    --   15.98  57.00-120.00   84
  4  \w    -53.00  85.00   1.00    1.00    --   15.98   0.00-150.00  138
  5  \w    -85.00   0.00   1.00    1.00    --  -17.23 -57.00   0.00   85
  6  \w    -20.00   7.00   1.00    1.00    --   15.98 -99.00  60.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0890618000
_diffrn_orient_matrix_UB_12      0.0166559000
_diffrn_orient_matrix_UB_13      0.0071326000
_diffrn_orient_matrix_UB_21      -0.0016599000
_diffrn_orient_matrix_UB_22      -0.0482028000
_diffrn_orient_matrix_UB_23      -0.0384565000
_diffrn_orient_matrix_UB_31      -0.0003743000
_diffrn_orient_matrix_UB_32      0.0336946000
_diffrn_orient_matrix_UB_33      -0.0373063000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0875
_diffrn_reflns_av_unetI/netI     0.1256
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14393
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.939
_diffrn_reflns_theta_min         3.491
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    1.550
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.064
_refine_diff_density_min         -2.503
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         6026
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0601
_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^)+0.3627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4562
_reflns_number_total             6026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01357f2.cif
_cod_data_source_block           lt170617-2
_cod_database_code               7710682
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 H1 O1 P1 Pt1'
_shelx_estimated_absorpt_t_max   0.404
_shelx_estimated_absorpt_t_min   0.216
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-H1A
 1 with sigma of 0.02
 B1-H1B
 0.95 with sigma of 0.02
 B1-H1C
 0.95 with sigma of 0.02
 B1-H1D
 0.95 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C4(H4)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C17(H17A,H17B,H17C), C12(H12A,H12B,H12C), C14(H14A,
 H14B,H14C), C10(H10A,H10B,H10C), C21(H21A,H21B,H21C), C9(H9A,H9B,H9C),
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              91053
_shelx_hkl_checksum              37399
_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 1.527
_oxdiff_exptl_absorpt_empirical_full_min 0.721