Synthesis and characterization of bis(pyrazolyl)borate Ni(ii) complexes: ligand rearrangement and transformation.
Zhao, Qianyi; Guan, Xin-Ting; Dou, Ting; Cao, Hou-Ji; Ma, Na-Na; Xu, Ting; Gao, Peng-Hui; Kong, Xiao-Hua; Zhang, Jie; Chen, Xuenian; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13242–13247; doi:10.1039/c9dt02287b

data_7700716
_publ_section_title
;
 Synthesis and characterization of bis(pyrazolyl)borate Ni(ii) complexes:
 ligand rearrangement and transformation.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13242
_journal_page_last               13247
_journal_paper_doi               10.1039/c9dt02287b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C32 H44 B2 Br4 N8 Ni, C3 H7'
_chemical_formula_sum            'C35 H51 B2 Br4 N8 Ni'
_chemical_formula_weight         983.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-23 deposited with the CCDC.    2019-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.2210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1521(2)
_cell_length_b                   19.2678(3)
_cell_length_c                   18.7249(2)
_cell_measurement_reflns_used    9212
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      71.0640
_cell_measurement_theta_min      4.2470
_cell_volume                     3932.36(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0528
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_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    -52.00  32.00   1.00    6.75    --  -35.37  57.00 -60.00   84
  2  \w   -103.00 -19.00   1.00    6.75    --  -35.37 -57.00  30.00   84
  3  \w   -103.00 -19.00   1.00    6.75    --  -35.37 -57.00 150.00   84
  4  \w      1.00  74.00   1.00    6.75    --   35.37 -99.00 120.00   73
  5  \w     19.00 103.00   1.00    6.75    --   35.37  57.00-120.00   84
  6  \w     23.00  89.00   1.00    6.75    --   35.37-125.00 -30.00   66
  7  \w     40.00 125.00   1.00   27.02    --  106.50 -61.00  90.00   85
  8  \w     37.00 109.00   1.00   27.02    --  106.50 -95.00-120.00   72
  9  \w     89.00 175.00   1.00   27.02    --  106.50  45.00-120.00   86
 10  \w     37.00  86.00   1.00   27.02    --  106.50 -95.00 120.00   49
 11  \w     43.00 100.00   1.00   27.02    --  106.50 -95.00  60.00   57
 12  \w     42.00 108.00   1.00   27.02    --  106.50 -95.00 -30.00   66
 13  \w    112.00 171.00   1.00   27.02    --  106.50  61.00  90.00   59
 14  \w     66.00 118.00   1.00   27.02    --  106.50 178.00   0.00   52
 15  \w     89.00 146.00   1.00   27.02    --  106.50  61.00-150.00   57
;
_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      -0.0679458000
_diffrn_orient_matrix_UB_12      0.0700513000
_diffrn_orient_matrix_UB_13      -0.0127172000
_diffrn_orient_matrix_UB_21      0.1198754000
_diffrn_orient_matrix_UB_22      0.0358721000
_diffrn_orient_matrix_UB_23      -0.0081438000
_diffrn_orient_matrix_UB_31      -0.0318434000
_diffrn_orient_matrix_UB_32      -0.0143336000
_diffrn_orient_matrix_UB_33      -0.0827306000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18596
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.257
_diffrn_reflns_theta_min         4.259
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.758
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       block
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.365
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         7491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0414P)^2^+6.0362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6779
_reflns_number_total             7491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02287b2.cif
_cod_data_source_block           gxt-201812-20
_cod_depositor_comments
'Adding full bibliography for 7700714--7700718.cif.'
_cod_database_code               7700716
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 H1 B1 N1 Ni1 Br1 '
_reflns_odcompleteness_completeness 99.96
_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 Ternary CH refined with riding coordinates:
 C1(H1), C5(H5), C9(H9), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B),
  C16(H16A,H16B), C00U(H00A,H00B), C019(H01D,H01E)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C21(H21), C25(H25), C29(H29)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C32(H32A,H32B,
 H32C), C01B(H01A,H01B,H01C)
;
_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 1.256
_oxdiff_exptl_absorpt_empirical_full_min 0.775