Development of a novel scorpionate ligand with 6-methylpyridine and comparison of structural and electronic properties of nickel(II) complexes with related tris(azolyl)borates
Fujiwara, Yusuke; Takayama, Tomoaki; Nakazawa, Jun; Okamura, Masaya; Hikichi, Shiro; Dalton Transactions  (2022) –; doi:10.1039/D2DT01548J

data_7710402
_publ_section_title
;
 Development of a novel scorpionate ligand with 6-methylpyridine and
 comparison of structural and electronic properties of nickel(II)
 complexes with related tris(azolyl)borates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01548J
_journal_year                    2022
_chemical_formula_moiety         'C24 H23 B Br N3 Ni'
_chemical_formula_sum            'C24 H23 B Br N3 Ni'
_chemical_formula_weight         502.88
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-05-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-05-16 deposited with the CCDC.	2022-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.906(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9893(2)
_cell_length_b                   15.9480(3)
_cell_length_c                   13.6069(3)
_cell_measurement_reflns_used    26442
_cell_measurement_temperature    90
_cell_measurement_theta_max      76.0760
_cell_measurement_theta_min      4.2400
_cell_volume                     2166.51(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.114a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.114a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.114a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      90.00
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_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     31.00 119.00   0.50    0.05    --   46.17  57.00  30.00  176
  2  \w     41.00  67.00   0.50    0.05    --   46.17  47.00-125.00   52
  3  \w     69.00 109.00   0.50    0.05    --   46.17  47.00-125.00   80
  4  \w    -12.00  14.00   0.50    0.05    --  -46.17  19.00  30.00   52
  5  \w     -8.00  29.00   0.50    0.05    --  -46.17  19.00   0.00   74
  6  \w    -18.00  28.00   0.50    0.05    --  -46.17  19.00 -30.00   92
  7  \w    -36.00 -11.00   0.50    0.05    --  -46.17  47.00-125.00   50
  8  \w     35.00  68.00   0.50    0.05    --  104.15 -61.00-150.00   66
  9  \w     36.00  71.00   0.50    0.05    --  104.15 -61.00 -90.00   70
 10  \w     39.00  74.00   0.50    0.05    --  104.15 -61.00 -60.00   70
 11  \w     42.00  67.00   0.50    0.05    --  104.15 -61.00 -30.00   50
 12  \w    -11.00  52.00   0.50    0.05    --   46.17 -47.00  85.00  126
 13  \w     32.00  79.00   0.50    0.05    --  104.15 -94.00 -90.00   94
 14  \w     21.00  93.00   0.50    0.05    --   46.17-125.00-150.00  144
 15  \w     37.00  74.00   0.50    0.05    --  104.15-125.00  30.00   74
 16  \w     94.00 120.00   0.50    0.05    --  104.15  47.00-125.00   52
 17  \w     84.00 110.00   0.50    0.05    --  104.15  77.00 -30.00   52
 18  \w    131.00 171.00   0.50    0.05    --  104.15  77.00 -30.00   80
 19  \w    108.00 175.00   0.50    0.05    --  104.15  45.00  30.00  134
 20  \w    125.00 171.00   0.50    0.05    --  104.15  61.00 150.00   92
 21  \w     89.00 115.00   0.50    0.05    --  104.15  61.00 150.00   52
 22  \w    -70.00 -31.00   0.50    0.05    -- -102.00  61.00-120.00   78
 23  \w    -66.00 -30.00   0.50    0.05    -- -102.00  61.00  60.00   72
 24  \w    -70.00 -38.00   0.50    0.05    -- -102.00  61.00  90.00   64
 25  \w    -69.00 -32.00   0.50    0.05    -- -102.00  61.00 120.00   74
 26  \w   -170.00-144.00   0.50    0.05    -- -102.00 -83.00  22.07   52
 27  \w   -175.00-128.00   0.50    0.05    -- -102.00 -77.00 -30.00   94
 28  \w   -105.00 -80.00   0.50    0.05    -- -102.00 -83.00  22.07   50
 29  \w   -109.00 -80.00   0.50    0.05    -- -102.00 -77.00  60.00   58
 30  \w   -104.00 -79.00   0.50    0.05    -- -102.00 -77.00  30.00   50
 31  \w   -107.00 -82.00   0.50    0.05    -- -102.00 -77.00   0.00   50
 32  \w   -105.00 -80.00   0.50    0.05    -- -102.00 -81.00 -16.54   50
 33  \w   -108.00 -80.00   0.50    0.05    -- -102.00 -77.00 -30.00   56
 34  \w   -175.00-132.00   0.50    0.05    -- -102.00 -77.00  30.00   86
 35  \w   -171.00-135.00   0.50    0.05    -- -102.00 -77.00   0.00   72
 36  \w   -121.00 -85.00   0.50    0.05    -- -102.00 -61.00  30.00   72
 37  \w    -92.00 -31.00   0.50    0.05    --  -46.17 -57.00   0.00  122
 38  \w   -108.00 -82.00   0.50    0.05    -- -102.00 -69.00 -22.44   52
 39  \w   -118.00 -87.00   0.50    0.05    -- -102.00 -59.00  11.77   62
 40  \w   -174.00 -85.00   0.50    0.05    -- -102.00 -61.00   0.00  178
 41  \w   -162.00 -87.00   0.50    0.05    -- -102.00 -57.00 -51.00  150
 42  \w   -113.00 -88.00   0.50    0.05    -- -102.00 -56.00 -45.49   50
 43  \w   -119.00 -93.00   0.50    0.05    -- -102.00 -49.00 -35.06   52
 44  \w   -155.00 -89.00   0.50    0.05    -- -102.00 -49.00 -30.98  132
 45  \w   -138.00 -87.00   0.50    0.05    -- -102.00 -55.00  14.03  102
 46  \w   -131.00 -92.00   0.50    0.05    -- -102.00 -47.00  85.00   78
 47  \w   -172.00 -91.00   0.50    0.05    -- -102.00 -45.00 150.00  162
 48  \w    -87.00 -61.00   0.50    0.05    --  -46.17 -47.00  85.00   52
 49  \w   -116.00 -91.00   0.50    0.05    -- -102.00 -53.00 -19.95   50
 50  \w   -164.00-105.00   0.50    0.05    -- -102.00 -45.00 -90.00  118
 51  \w   -172.00 -85.00   0.50    0.05    -- -102.00 -61.00-180.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32868
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.124
_diffrn_reflns_theta_min         4.272
_exptl_absorpt_coefficient_mu    3.562
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.114a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0307P)^2^+2.1093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4290
_reflns_number_total             4406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01548j2.cif
_cod_data_source_block           '[NiBr(TpyMe)]'
_cod_database_code               7710402
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.702
_shelx_estimated_absorpt_t_min   0.477
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C14(H14), C4(H4), C2(H2), C20(H20), C9(H9), C18(H18),
 C19(H19), C3(H3), C8(H8), C7(H7)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              76414
_shelx_hkl_checksum              79584
_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
;