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_7700715
_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 H48 B2 N8 Ni'
_chemical_formula_sum            'C32 H48 B2 N8 Ni'
_chemical_formula_weight         625.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2019-05-23 deposited with the CCDC.    2019-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                87.799(4)
_cell_angle_beta                 79.365(5)
_cell_angle_gamma                68.035(6)
_cell_formula_units_Z            1
_cell_length_a                   7.5038(5)
_cell_length_b                   9.7847(5)
_cell_length_c                   11.3835(6)
_cell_measurement_reflns_used    3062
_cell_measurement_temperature    295.2(4)
_cell_measurement_theta_max      71.9660
_cell_measurement_theta_min      4.8640
_cell_volume                     761.39(8)
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.2(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0528
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.973
_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      9.00 104.00   1.00    5.00    --   36.07  77.00 -60.00   95
  2  \w    -31.00  53.00   1.00    5.00    --   36.07 -57.00 -90.00   84
  3  \w      9.00 104.00   1.00    5.00    --   36.07  77.00 -30.00   95
  4  \w     19.00 103.00   1.00    5.00    --   36.07  57.00-120.00   84
  5  \w     23.00  89.00   1.00    5.00    --   36.07-125.00 150.00   66
  6  \w      9.00 104.00   1.00    5.00    --   36.07  77.00-180.00   95
  7  \w     23.00  89.00   1.00    5.00    --   36.07-125.00 -90.00   66
  8  \w     23.00  89.00   1.00    5.00    --   36.07-125.00 -60.00   66
  9  \w     23.00  89.00   1.00    5.00    --   36.07-125.00  60.00   66
 10  \w     17.00 105.00   1.00    5.00    --   36.07  38.00-180.00   88
 11  \w    -35.00  65.00   1.00    5.00    --   36.07 -19.00   0.00  100
 12  \w     23.00  89.00   1.00    5.00    --   36.07-125.00  90.00   66
 13  \w     92.00 178.00   1.00   11.00    --  109.31  45.00 120.00   86
 14  \w     40.00 109.00   1.00   11.00    --  109.31 -95.00  30.00   69
 15  \w     42.00 127.00   1.00   11.00    --  109.31 -61.00 -60.00   85
 16  \w     91.00 176.00   1.00   11.00    --  109.31  61.00 -90.00   85
 17  \w     91.00 176.00   1.00   11.00    --  109.31  61.00   0.00   85
 18  \w     40.00 109.00   1.00   11.00    --  109.31 -95.00 -90.00   69
 19  \w     40.00 109.00   1.00   11.00    --  109.31 -95.00 120.00   69
 20  \w     39.00 116.00   1.00   11.00    --  109.31-111.00-150.00   77
 21  \w     83.00 177.00   1.00   11.00    --  109.31  77.00  30.00   94
 22  \w     38.00 148.00   1.00   11.00    --  109.31 -15.00  90.00  110
 23  \w     42.00 127.00   1.00   11.00    --  109.31 -61.00 120.00   85
 24  \w    100.00 178.00   1.00   11.00    --  109.31 111.00-150.00   78
 25  \w     41.00 127.00   1.00   11.00    --  109.31 -45.00-150.00   86
 26  \w     19.00  88.00   1.00    5.00    --   36.07  57.00  60.00   69
;
_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      0.1295668000
_diffrn_orient_matrix_UB_12      0.0804335000
_diffrn_orient_matrix_UB_13      -0.0649205000
_diffrn_orient_matrix_UB_21      0.1359807000
_diffrn_orient_matrix_UB_22      -0.0544002000
_diffrn_orient_matrix_UB_23      0.0922436000
_diffrn_orient_matrix_UB_31      0.1242497000
_diffrn_orient_matrix_UB_32      -0.1393733000
_diffrn_orient_matrix_UB_33      -0.0791120000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7107
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.525
_diffrn_reflns_theta_min         3.953
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.200
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75797
_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            orange
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       plate
_exptl_crystal_F_000             334
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+0.4086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1239
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2562
_reflns_number_total             2935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02287b2.cif
_cod_data_source_block           gxt170912
_cod_depositor_comments
'Adding full bibliography for 7700714--7700718.cif.'
_cod_database_code               7700715
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 N1 B1 H1 Ni1'
_reflns_odcompleteness_completeness 99.74
_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:
 C5(H5), C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C9(H9), C13(H13), C10(H10)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C)
;
_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 1.433
_oxdiff_exptl_absorpt_empirical_full_min 0.710