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_7700718
_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         'C40 H66 B2 N8 Ni O'
_chemical_formula_sum            'C40 H65 B2 N8 Ni O'
_chemical_formula_weight         754.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-16
_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                 90.9030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.00180(10)
_cell_length_b                   10.8736(2)
_cell_length_c                   34.0677(3)
_cell_measurement_reflns_used    8667
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.4360
_cell_measurement_theta_min      3.9890
_cell_volume                     4074.98(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.42a (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_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    -73.00  34.00   1.00    2.19    --  -40.64  74.00 141.00  107
  2  \w     72.00 178.00   1.00    8.76    --  103.55  74.00 141.00  106
  3  \w     29.00 135.00   1.00    8.76    --  103.55 -74.00  13.00  106
  4  \w   -116.00  -9.00   1.00    2.19    --  -40.64 -74.00  13.00  107
  5  \w      1.00  82.00   1.00    2.19    --   40.64 -99.00-150.00   81
  6  \w     23.00  97.00   1.00    2.19    --   40.64-125.00 -60.00   74
  7  \w     27.00 112.00   1.00    8.76    --  103.55-111.00-150.00   85
  8  \w    100.00 143.00   1.00    8.76    --  103.55 111.00  30.00   43
  9  \w     34.00  80.00   1.00    8.76    --  103.55 -45.00  60.00   46
 10  \w     48.00  74.00   1.00    8.76    --  103.55-111.00  30.00   26
 11  \w     89.00 128.00   1.00    8.76    --  103.55 -45.00  60.00   39
 12  \w     27.00 102.00   1.00    8.76    --  103.55-111.00   0.00   75
 13  \w     86.00 112.00   1.00    8.76    --  103.55-111.00  30.00   26
 14  \w    115.00 168.00   1.00    8.76    --  103.55 111.00  60.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0983933000
_diffrn_orient_matrix_UB_12      -0.0255604000
_diffrn_orient_matrix_UB_13      0.0306460000
_diffrn_orient_matrix_UB_21      0.0719146000
_diffrn_orient_matrix_UB_22      -0.1130573000
_diffrn_orient_matrix_UB_23      0.0145953000
_diffrn_orient_matrix_UB_31      0.0690315000
_diffrn_orient_matrix_UB_32      0.0814256000
_diffrn_orient_matrix_UB_33      0.0298896000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            22863
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.335
_diffrn_reflns_theta_min         4.019
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.42a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.745
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         7846
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0621
_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^)+(0.1001P)^2^+6.8451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.1869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6257
_reflns_number_total             7846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02287b2.cif
_cod_data_source_block           gxt-0429-1
_cod_depositor_comments
'Adding full bibliography for 7700714--7700718.cif.'
_cod_original_cell_volume        4074.99(9)
_cod_database_code               7700718
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 H1 N1 Ni1 B1 '
_diffrn_oxdiff_digest_frames
;
0159dbb991febdd638cacf045d4167384a00030aafb
;
_diffrn_oxdiff_digest_hkl
;
01e45a367b7b32dcf6cb50a65c1aa55c510fcc
;
_reflns_odcompleteness_completeness 99.95
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 B2-H1
 1.966644 with sigma of 0.02
 Ni1-H1
 2.648021 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C13(H13), C9(H9), C5(H5), C22(H22), C26(H26), C32(H32), C1(H1A), C38(H38)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C4(H4A,H4B), C10(H10A,H10B), C12(H12A,H12B),
 C16(H16A,H16B), C6(H6A,H6B), C11(H11A,H11B), C3(H3A,H3B), C8(H8A,H8B), C7(H7A,
 H7B), C2(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 N8(H8), C25(H25), C24(H24), C18(H18), C19(H19), C31(H31), C30(H30), C37(H37),
 C36(H36)
3.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C27(H27A,H27B,H27C), C33(H33A,H33B,H33C), C20(H20A,H20B,
 H20C), C40(H40A,H40B,H40C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C39(H39A,
 H39B,H39C)
;
_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 1.415
_oxdiff_exptl_absorpt_empirical_full_min 0.253