The crystal structure of nitroxyl-κ N-{hydridotris(3-trifluoromethyl-5-methylpyrazolyl-1-yl-κN 3)borato}nickel(II), C15H13BF9N7NiO
Fujisawa, Kiyoshi; Kataoka, Taisei; Terashima, Kohei; Tiekink, Edward R. T.; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 1075–1078; doi:10.1515/ncrs-2022-0369

data_8107297
_publ_section_title
;
 The crystal structure of nitroxyl-\k
 N-{hydridotris(3-trifluoromethyl-5-methylpyrazolyl-1-yl-\kN
 3)borato}nickel(II), C15H13BF9N7NiO
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1075
_journal_page_last               1078
_journal_paper_doi               10.1515/ncrs-2022-0369
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C15 H13 B F9 N7 Ni O'
_chemical_formula_sum            'C15 H13 B F9 N7 Ni O'
_chemical_formula_weight         547.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8513(3)
_cell_length_b                   13.3869(2)
_cell_length_c                   8.5944(2)
_cell_measurement_reflns_used    22066
_cell_measurement_temperature    124(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     2053.83(7)
_computing_cell_refinement       'CrysAlis^PRO^ [1]'
_computing_data_collection       'CrysAlis^PRO^ [1]'
_computing_data_reduction        'CrysAlis^PRO^ [1]'
_computing_molecular_graphics    'ORTEP-3 for Windows [4]'
_computing_publication_material  'SHELXL-2018/3 [3]'
_computing_structure_refinement  'SHELXL-2018/3 [3]'
_computing_structure_solution    'SIR2014 [2]'
_diffrn_ambient_temperature      124(2)
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0076
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            32121
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.630
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis^PRO^ [1]
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0414P)^2^+0.7537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2314
_reflns_number_total             2455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0369_suppl.cif
_cod_data_source_block           shelx
_cod_database_code               8107297
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.907
_shelx_estimated_absorpt_t_max   0.958
_shelx_res_checksum              44743
_shelx_hkl_checksum              89653