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_7700717
_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      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             2017-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-05-23 deposited with the CCDC.    2019-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.950(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8173(4)
_cell_length_b                   24.0412(10)
_cell_length_c                   15.2894(9)
_cell_measurement_reflns_used    4529
_cell_measurement_temperature    293.99(18)
_cell_measurement_theta_max      25.7710
_cell_measurement_theta_min      4.0990
_cell_volume                     3217.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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      293.99(18)
_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 0.997
_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     35.00  88.00   1.00   19.42    --   15.98 178.00 -60.00   53
  2  \w     -1.00  39.00   1.00   19.42    --   15.98  57.00 150.00   40
  3  \w    -52.00 -26.00   1.00   19.42    --   15.98 -19.00  60.00   26
  4  \w    -14.00  44.00   1.00   19.42    --   15.98 -19.00  60.00   58
  5  \w    -47.00  43.00   1.00   19.42    --   15.98 -77.00  30.00   90
;
_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      -0.0672235000
_diffrn_orient_matrix_UB_12      0.0126769000
_diffrn_orient_matrix_UB_13      -0.0212895000
_diffrn_orient_matrix_UB_21      0.0391904000
_diffrn_orient_matrix_UB_22      0.0257314000
_diffrn_orient_matrix_UB_23      -0.0007024000
_diffrn_orient_matrix_UB_31      0.0226975000
_diffrn_orient_matrix_UB_32      -0.0069136000
_diffrn_orient_matrix_UB_33      -0.0415856000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15648
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.390
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0455
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4572
_reflns_number_total             5657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02287b2.cif
_cod_data_source_block           gxt-20171119-ni
_cod_depositor_comments
'Adding full bibliography for 7700714--7700718.cif.'
_cod_database_code               7700717
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 B1 N1 H1 Ni1 '
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C9(H9), C13(H13), C5(H5), C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C4(H4A,H4B), C15(H15A,H15B), C14(H14A,H14B), C8(H8A,H8B),
 C10(H10A,H10B), C7(H7A,H7B), C2(H2A,H2B), C12(H12A,H12B), C6(H6A,H6B),
 C11(H11A,H11B), C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C25(H25), C17(H17), C21(H21), C18(H18), C26(H26), C30(H30), C29(H29)
2.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C20(H20A,H20B,
 H20C)
;
_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 1.688
_oxdiff_exptl_absorpt_empirical_full_min 0.634