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_7710399
_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 Cl N3 Ni'
_chemical_formula_sum            'C24 H23 B Cl N3 Ni'
_chemical_formula_weight         458.42
_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   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                 90.3207(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.03974(17)
_cell_length_b                   15.8652(2)
_cell_length_c                   13.3756(2)
_cell_measurement_reflns_used    9579
_cell_measurement_temperature    90
_cell_measurement_theta_max      76.5980
_cell_measurement_theta_min      5.5030
_cell_volume                     2130.47(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (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 0.968
_diffrn_measured_fraction_theta_max 0.927
_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    100.00 132.00   0.50    0.20    --  104.75  15.00  30.00   64
  2  \w     99.00 170.00   0.50    0.20    --  104.75  15.00 120.00  142
  3  \w    144.00 173.00   0.50    0.20    --  104.75  15.00  30.00   58
  4  \w     58.00 107.00   0.50    0.05    --   46.27  65.00-176.00   98
  5  \w    -14.00  24.00   0.50    0.05    --  -46.27  19.00  60.00   76
  6  \w    -60.00 -32.00   0.50    0.20    -- -102.00  61.00  30.00   56
  7  \w   -160.00-111.00   0.50    0.20    -- -102.00 -69.00 -84.00   98
  8  \w    -55.00 -30.00   0.50    0.20    -- -102.00  61.00-180.00   50
  9  \w    -93.00 -14.00   0.50    0.05    --  -46.27 125.00  60.00  158
 10  \w     37.00  62.00   0.50    0.20    --  104.75 -45.00 -90.00   50
 11  \w     33.00  58.00   0.50    0.20    --  104.75 -45.00 -60.00   50
 12  \w     34.00  60.00   0.50    0.20    --  104.75 -45.00-120.00   52
 13  \w     33.00  58.00   0.50    0.20    --  104.75 -45.00-180.00   50
 14  \w    -25.00  66.00   0.50    0.05    --   46.27 -69.00 -84.00  182
 15  \w     52.00  77.00   0.50    0.20    --  104.75 -65.00  48.00   50
 16  \w     37.00  92.00   0.50    0.20    --  104.75-125.00 150.00  110
 17  \w     32.00 105.00   0.50    0.20    --  104.75 -89.00 172.00  146
 18  \w     75.00 105.00   0.50    0.20    --  104.75 -94.00  90.00   60
 19  \w     32.00 105.00   0.50    0.20    --  104.75 -94.00 -90.00  146
;
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12755
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.791
_diffrn_reflns_theta_min         4.323
_exptl_absorpt_coefficient_mu    2.578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (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    1.429
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0403P)^2^+0.6793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3755
_reflns_number_total             4165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01548j2.cif
_cod_data_source_block           '[NiCl(TpyMe)]'
_cod_database_code               7710399
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.701
_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:
 C9(H9), C8(H8), C7(H7), C21(H21), C17(H17), C20(H20), C14(H14), C4(H4),
 C2(H2), C19(H19), C3(H3), C18(H18), C13(H13), C12(H12)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              95630
_shelx_hkl_checksum              36233
_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
;