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_7710400
_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         'C20 H23 B Cl2 Co N2 O'
_chemical_formula_sum            'C20 H23 B Cl2 Co N2 O'
_chemical_formula_weight         448.04
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-01-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2022-05-16 deposited with the CCDC.	2022-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.356(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3720(2)
_cell_length_b                   26.7621(6)
_cell_length_c                   11.1119(3)
_cell_measurement_reflns_used    17438
_cell_measurement_temperature    90
_cell_measurement_theta_max      76.2530
_cell_measurement_theta_min      3.2230
_cell_volume                     2080.72(10)
_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 1.000
_diffrn_measured_fraction_theta_max 0.974
_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     98.00 171.00   0.50    0.05    --  104.15  45.00 150.00  146
  2  \w    103.00 129.00   0.50    0.05    --  104.15  45.00 -30.00   52
  3  \w    109.00 149.00   0.50    0.05    --  104.15  75.00-150.00   80
  4  \w     57.00 102.00   0.50    0.05    --   46.17  75.00-150.00   90
  5  \w    -62.00  -5.00   0.50    0.05    --  -46.17  75.00-150.00  114
  6  \w    -19.00  23.00   0.50    0.05    --  -46.17  19.00-180.00   84
  7  \w    -18.00  29.00   0.50    0.05    --  -46.17  19.00-150.00   94
  8  \w    -19.00  29.00   0.50    0.05    --  -46.17  19.00   0.00   96
  9  \w    -59.00   8.00   0.50    0.05    --  -46.17  57.00  60.00  134
 10  \w    -13.00  28.00   0.50    0.05    --  -46.17  19.00 120.00   82
 11  \w    -19.00  29.00   0.50    0.05    --  -46.17  19.00  90.00   96
 12  \w    -90.00 -65.00   0.50    0.05    -- -102.00  75.00-150.00   50
 13  \w    -67.00 -29.00   0.50    0.05    -- -102.00  61.00-180.00   76
 14  \w    -62.00 -29.00   0.50    0.05    -- -102.00  61.00 -90.00   66
 15  \w    -68.00 -31.00   0.50    0.05    -- -102.00  61.00  30.00   74
 16  \w    -70.00 -29.00   0.50    0.05    -- -102.00  61.00  60.00   82
 17  \w    -64.00 -34.00   0.50    0.05    -- -102.00  61.00  90.00   60
 18  \w    -62.00 -29.00   0.50    0.05    -- -102.00 125.00  30.00   66
 19  \w   -104.00 -74.00   0.50    0.05    -- -102.00 125.00  30.00   60
 20  \w   -116.00 -91.00   0.50    0.05    -- -102.00 -61.00   0.00   50
 21  \w   -169.00-129.00   0.50    0.05    -- -102.00 -61.00   0.00   80
 22  \w   -172.00 -89.00   0.50    0.05    -- -102.00 -45.00 -60.00  166
 23  \w   -171.00 -90.00   0.50    0.05    -- -102.00 -45.00 -30.00  162
 24  \w   -154.00 -89.00   0.50    0.05    -- -102.00 -15.00 -30.00  130
 25  \w   -173.00 -89.00   0.50    0.05    -- -102.00 -30.00  30.00  168
 26  \w   -154.00-118.00   0.50    0.05    -- -102.00 -75.00  81.00   72
 27  \w    -95.00 -70.00   0.50    0.05    --  -46.17 -75.00  81.00   50
 28  \w    -23.00  22.00   0.50    0.05    --   46.17 -19.00-180.00   90
 29  \w     36.00  73.00   0.50    0.05    --  104.15 -77.00-150.00   74
 30  \w     85.00 127.00   0.50    0.05    --  104.15 -77.00-150.00   84
 31  \w    -23.00  39.00   0.50    0.05    --   46.17 -75.00  81.00  124
 32  \w     33.00  75.00   0.50    0.05    --  104.15 -75.00  81.00   84
 33  \w     79.00 108.00   0.50    0.05    --  104.15 -75.00  81.00   58
 34  \w     35.00  75.00   0.50    0.05    --  104.15 -61.00  90.00   80
 35  \w     47.00 106.00   0.50    0.05    --  104.15 -94.00 -30.00  118
 36  \w     71.00 105.00   0.50    0.05    --  104.15 -94.00 -90.00   68
 37  \w     33.00 103.00   0.50    0.05    --  104.15-125.00 -90.00  140
 38  \w     39.00  64.00   0.50    0.05    --  104.15-125.00-120.00   50
 39  \w     51.00  86.00   0.50    0.05    --  104.15 -94.00-180.00   70
 40  \w     81.00 106.00   0.50    0.05    --  104.15-125.00-120.00   50
 41  \w     37.00  63.00   0.50    0.05    --  104.15 -94.00  30.00   52
 42  \w     75.00 102.00   0.50    0.05    --  104.15 -94.00  30.00   54
;
_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  0.0336
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27044
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.516
_diffrn_reflns_theta_min         3.303
_exptl_absorpt_coefficient_mu    8.917
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74143
_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 blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.289
_exptl_crystal_size_min          0.266
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0338P)^2^+2.2650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4157
_reflns_number_total             4250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01548j2.cif
_cod_data_source_block           '[CoCl2[PhB(OEt)(pyMe)(HpyMe)]]'
_cod_database_code               7710400
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.200
_shelx_estimated_absorpt_t_min   0.128
_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
2.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2A), C4(H4), C12(H12), C3(H3), C14(H14), C13(H13), C16(H16),
 C15(H15), C9(H9), C7(H7), C8(H8)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              48806
_shelx_hkl_checksum              76399
_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
;