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_7710398
_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 H24 B N3'
_chemical_formula_sum            'C24 H24 B N3'
_chemical_formula_weight         365.27
_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                 101.238(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1227(4)
_cell_length_b                   9.2714(3)
_cell_length_c                   16.9147(5)
_cell_measurement_reflns_used    24739
_cell_measurement_temperature    90
_cell_measurement_theta_max      76.5110
_cell_measurement_theta_min      3.9440
_cell_volume                     2018.48(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.106a (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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_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     27.00  53.00   0.50    0.05    --   46.56  77.00   0.00   52
  2  \w     24.00  53.00   0.50    0.05    --   46.56  77.00 -30.00   58
  3  \w     29.00  54.00   0.50    0.05    --   46.56  77.00 -60.00   50
  4  \w     24.00  58.00   0.50    0.05    --   46.56  77.00 -90.00   68
  5  \w     32.00  66.00   0.50    0.05    --   46.56  57.00 -90.00   68
  6  \w     24.00  50.00   0.50    0.05    --   46.56  77.00-120.00   52
  7  \w     33.00  88.00   0.50    0.05    --   46.56  57.00-180.00  110
  8  \w     34.00  70.00   0.50    0.05    --   46.56  57.00-150.00   72
  9  \w     38.00  67.00   0.50    0.05    --   46.56  57.00-120.00   58
 10  \w     35.00  60.00   0.50    0.05    --   46.56  37.00 -90.00   50
 11  \w     44.00  81.00   0.50    0.05    --   46.56  19.00 -90.00   74
 12  \w     37.00  63.00   0.50    0.05    --   46.56   6.00-177.00   52
 13  \w    -10.00  24.00   0.50    0.05    --  -46.56   6.00-177.00   68
 14  \w    -54.00 -29.00   0.50    0.11    -- -102.00 109.00-102.91   50
 15  \w   -108.00 -70.00   0.50    0.11    -- -102.00 109.00-102.91   76
 16  \w     82.00 107.00   0.50    0.11    --  104.62  77.00-180.00   50
 17  \w    118.00 144.00   0.50    0.11    --  104.62   6.00-177.00   52
 18  \w    -25.00  24.00   0.50    0.05    --   46.56 -19.00 -90.00   98
 19  \w    -24.00   1.00   0.50    0.05    --   46.56  -6.00   5.00   50
 20  \w     66.00 108.00   0.50    0.11    --  104.62 -77.00-120.00   84
 21  \w     33.00  75.00   0.50    0.11    --  104.62 -61.00 -60.00   84
 22  \w     37.00  62.00   0.50    0.11    --  104.62 -77.00-120.00   50
 23  \w     32.00  75.00   0.50    0.11    --  104.62 -61.00-120.00   86
 24  \w     48.00  75.00   0.50    0.11    --  104.62 -94.00-180.00   54
 25  \w     78.00 104.00   0.50    0.11    --  104.62 -94.00-180.00   52
 26  \w     36.00 103.00   0.50    0.11    --  104.62 -94.00-150.00  134
 27  \w     18.00  91.00   0.50    0.05    --   46.56-125.00-180.00  146
 28  \w   -112.00 -70.00   0.50    0.05    --  -46.56  -6.00   5.00   84
 29  \w   -104.00 -79.00   0.50    0.11    -- -102.00 -77.00 -60.00   50
 30  \w   -105.00 -79.00   0.50    0.11    -- -102.00 -77.00 -90.00   52
 31  \w   -106.00 -81.00   0.50    0.11    -- -102.00 -77.00-112.01   50
 32  \w   -104.00 -79.00   0.50    0.11    -- -102.00 -77.00-150.00   50
 33  \w   -104.00 -79.00   0.50    0.11    -- -102.00 -77.00-180.00   50
 34  \w   -150.00-124.00   0.50    0.11    -- -102.00 -77.00-150.00   52
 35  \w   -169.00-143.00   0.50    0.11    -- -102.00 -77.00 -90.00   52
 36  \w   -104.00 -79.00   0.50    0.11    -- -102.00 -76.00-122.75   50
 37  \w   -104.00 -79.00   0.50    0.11    -- -102.00 -76.00 -82.12   50
 38  \w   -105.00 -80.00   0.50    0.11    -- -102.00 -77.00 -30.00   50
 39  \w   -105.00 -80.00   0.50    0.11    -- -102.00 -74.00 -29.97   50
 40  \w   -104.00 -79.00   0.50    0.11    -- -102.00 -76.00   2.90   50
 41  \w   -108.00 -83.00   0.50    0.11    -- -102.00 -77.00   0.00   50
 42  \w   -109.00 -82.00   0.50    0.11    -- -102.00 -71.00 -58.05   54
 43  \w   -107.00 -82.00   0.50    0.11    -- -102.00 -72.00-111.33   50
 44  \w   -174.00 -82.00   0.50    0.11    -- -102.00 -71.00-103.93  184
 45  \w   -173.00-147.00   0.50    0.11    -- -102.00 -76.00   2.90   52
 46  \w   -175.00-149.00   0.50    0.11    -- -102.00 -74.00 -29.97   52
 47  \w   -174.00-148.00   0.50    0.11    -- -102.00 -68.00 -24.63   52
 48  \w   -162.00-136.00   0.50    0.11    -- -102.00 -71.00 -58.05   52
 49  \w   -109.00 -84.00   0.50    0.11    -- -102.00 -66.00 -32.89   50
 50  \w   -108.00 -83.00   0.50    0.11    -- -102.00 -68.00 -24.63   50
 51  \w   -109.00 -84.00   0.50    0.11    -- -102.00 -64.00 -57.37   50
 52  \w   -114.00 -85.00   0.50    0.11    -- -102.00 -64.00 -91.02   58
 53  \w   -110.00 -85.00   0.50    0.11    -- -102.00 -63.00 -84.78   50
 54  \w   -108.00 -83.00   0.50    0.11    -- -102.00 -68.00-147.89   50
 55  \w   -108.00 -83.00   0.50    0.11    -- -102.00 -67.00-169.30   50
 56  \w   -110.00 -85.00   0.50    0.11    -- -102.00 -61.00-150.00   50
 57  \w   -164.00 -87.00   0.50    0.11    -- -102.00 -56.00-169.60  154
 58  \w   -175.00 -84.00   0.50    0.11    -- -102.00 -64.00-120.68  182
 59  \w   -151.00 -90.00   0.50    0.11    -- -102.00 -61.00 -90.00  122
 60  \w   -112.00 -87.00   0.50    0.11    -- -102.00 -61.00 -30.00   50
 61  \w   -112.00 -87.00   0.50    0.11    -- -102.00 -57.00 -14.03   50
 62  \w   -113.00 -88.00   0.50    0.11    -- -102.00 -54.00 -30.25   50
 63  \w   -174.00 -88.00   0.50    0.11    -- -102.00 -48.00 -20.71  172
 64  \w   -173.00 -88.00   0.50    0.11    -- -102.00 -53.00 -34.41  170
 65  \w   -132.00 -94.00   0.50    0.11    -- -102.00 -47.00 -66.79   76
 66  \w   -150.00-125.00   0.50    0.11    -- -102.00  -6.00   5.00   50
 67  \w    -88.00 -35.00   0.50    0.05    --  -46.56 -43.00-119.77  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1149312000
_diffrn_orient_matrix_UB_12      -0.0006459000
_diffrn_orient_matrix_UB_13      -0.0081327000
_diffrn_orient_matrix_UB_21      0.0334011000
_diffrn_orient_matrix_UB_22      0.0127392000
_diffrn_orient_matrix_UB_23      0.0923326000
_diffrn_orient_matrix_UB_31      0.0019217000
_diffrn_orient_matrix_UB_32      -0.1654389000
_diffrn_orient_matrix_UB_33      0.0072542000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33233
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.352
_diffrn_reflns_theta_min         3.915
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.106a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.7212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3795
_reflns_number_total             4095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01548j2.cif
_cod_data_source_block           HTpyMe
_cod_database_code               7710398
_shelx_shelxl_version_number     2018/3
_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), C3(H3), C21(H21), C2(H2), C15(H15), C16(H16), C17(H17), C11(H11),
 C25(H25), C24(H24), C23(H23), C22(H22), C4(H4), C10(H10)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              34160
_shelx_hkl_checksum              24071
_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 1.203
_oxdiff_exptl_absorpt_empirical_full_min 0.870