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_7710401
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C21 H29 B Br N3 Ni O3'
_chemical_formula_sum            'C21 H29 B Br N3 Ni O3'
_chemical_formula_weight         520.90
_chemical_name_common
'[bromo(Phenyltris(oxiazolynyl)borato)nickel(II)]'
_chemical_name_systematic        Ni(Ph-To)Br
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-05-16 deposited with the CCDC.	2022-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.895(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0336(5)
_cell_length_b                   13.2310(4)
_cell_length_c                   16.0271(10)
_cell_measurement_reflns_used    6804
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.4831
_cell_measurement_theta_min      1.8555
_cell_volume                     2327.35(19)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction
'CrystalClear (Rigaku Inc., 2007), SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
scan:
	Number of images: 600
	           Slice: -110.0000 - 70.0000
	     Image width: 0.3000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 44.8414
	          2theta: -20.1817
scan:
	Number of images: 600
	           Slice: -110.0000 - 70.0000
	     Image width: 0.3000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 44.8414
	          2theta: -20.1817

;
_diffrn_measurement_device
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       \w
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0014
_diffrn_orient_matrix_UB_12      0.0002
_diffrn_orient_matrix_UB_13      -0.0911
_diffrn_orient_matrix_UB_21      -0.0547
_diffrn_orient_matrix_UB_22      -0.0522
_diffrn_orient_matrix_UB_23      0.0007
_diffrn_orient_matrix_UB_31      -0.0432
_diffrn_orient_matrix_UB_32      0.0451
_diffrn_orient_matrix_UB_33      -0.0056
_diffrn_radiation_detector       CCD
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5439
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.4831
_diffrn_reflns_theta_max         27.4831
_diffrn_reflns_theta_min         1.8555
_diffrn_source_current           60.0000
_diffrn_source_power             3.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.577
_exptl_absorpt_correction_T_max  0.7758
_exptl_absorpt_correction_T_min  0.5855
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;Numerical (Based on real shape of the crystal) absorption
correction was parformed on CrystalClear (Rigaku Inc., 2007)
with FS_ABSCOR method.
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       Block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0270P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4137
_reflns_number_total             5213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01548j2.cif
_cod_data_source_block           '[NiBr(ToM)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Numerical' was
changed to 'numerical' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7710401
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.425
_shelx_estimated_absorpt_t_max   0.783
_diffrn_number_total             5439
_diffrn_reflns_av_sigmai/deti    0.0610
_shelx_res_checksum              64161
_shelx_hkl_checksum              13217