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_7710684
_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 Ni P2'
_chemical_formula_sum            'C24 H48 B2 N2 Ni P2'
_chemical_formula_weight         506.91
_chemical_name_systematic        tBu-PBP-Ni-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                   11.67670(10)
_cell_length_b                   14.53350(10)
_cell_length_c                   32.1537(3)
_cell_measurement_reflns_used    13325
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      71.5380
_cell_measurement_theta_min      4.0930
_cell_volume                     5456.59(8)
_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      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.981
_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    -75.00  20.00   1.00    1.00    --  -35.62  99.00  18.00   95
  2  \w    -32.00  52.00   1.00    1.00    --   35.62 -55.00 140.00   84
  3  \w      1.00  75.00   1.00    1.00    --   35.62 -99.00 -88.00   74
  4  \w     82.00 174.00   1.00    1.11    --  107.12  74.00 133.00   92
  5  \w     40.00 124.00   1.00    1.11    --  107.12 -55.00 140.00   84
  6  \w     37.00 110.00   1.00    1.11    --  107.12 -99.00 -88.00   73
  7  \w    -52.00  32.00   1.00    1.00    --  -35.62  57.00-180.00   84
  8  \w     55.00 108.00   1.00    1.00    --   35.62-178.00  30.00   53
  9  \w     57.00 108.00   1.00    1.00    --   35.62 178.00-150.00   51
 10  \w     40.00 125.00   1.00    1.11    --  107.12 -61.00 -90.00   85
 11  \w    103.00 170.00   1.00    1.11    --  107.12 111.00 -60.00   67
 12  \w     74.00 105.00   1.00    1.11    --  107.12 -95.00 -30.00   31
 13  \w     83.00 127.00   1.00    1.11    --  107.12 -30.00 -30.00   44
;
_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      0.0380031000
_diffrn_orient_matrix_UB_12      -0.0823143000
_diffrn_orient_matrix_UB_13      0.0268680000
_diffrn_orient_matrix_UB_21      0.1009070000
_diffrn_orient_matrix_UB_22      0.0571194000
_diffrn_orient_matrix_UB_23      0.0169852000
_diffrn_orient_matrix_UB_31      -0.0761111000
_diffrn_orient_matrix_UB_32      0.0345990000
_diffrn_orient_matrix_UB_33      0.0358293000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_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       -27
_diffrn_reflns_number            20816
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.505
_diffrn_reflns_theta_min         4.680
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.219
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85520
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0439P)^2^+2.6853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4754
_reflns_number_total             5212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01357f2.cif
_cod_data_source_block           dyz20191107
_cod_database_code               7710684
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 B1 N1 P1 Ni1'
_shelx_estimated_absorpt_t_max   0.792
_shelx_estimated_absorpt_t_min   0.761
_diffrn_oxdiff_digest_frames
;
018333c913e2d497252726c8d6951c702a00957f907
;
_diffrn_oxdiff_digest_hkl
;
011ba7e8b4e08dbe1ae0013877ab8cc45f0852
;
_reflns_odcompleteness_completeness 99.87
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C6(H6), C5(H5)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C11(H11A,H11B,
 H11C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C10(H10A,H10B,H10C), C12(H12A,
 H12B,H12C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C),
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              74766
_shelx_hkl_checksum              8476
_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 1.271
_oxdiff_exptl_absorpt_empirical_full_min 0.606