A tetragonal polymorph of bis[hydrotris(pyrazol-1-yl)borato]iron(II)
Ni, Zhong-Hai; Li, Guo-Ling; Ma, Rui; Nie, Jing; Acta Crystallographica Section E 67 (2011) m1033–; doi:10.1107/S1600536811025839

data_2231141
_publ_section_title
;
 A tetragonal polymorph of bis[hydrotris(pyrazol-1-yl)borato]iron(II)
;
_journal_coeditor_code           HG5058
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1033
_journal_paper_doi               10.1107/S1600536811025839
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Fe (C9 H10 B1 N6)2]'
_chemical_formula_moiety         'C18 H20 B2 Fe N12'
_chemical_formula_sum            'C18 H20 B2 Fe N12'
_chemical_formula_weight         481.93
_chemical_name_systematic
;
bis[hydrotris(pyrazol-1-yl)borato]iron(II)
;
_space_group_IT_number           138
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4ac 2ac'
_symmetry_space_group_name_H-M   'P 42/n c m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.017(3)
_cell_length_b                   17.017(3)
_cell_length_c                   7.4099(15)
_cell_measurement_reflns_used    1210
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      2.38
_cell_volume                     2145.7(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XP (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14091
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.39
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.386
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+2.7074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1226
_reflns_number_gt                1095
_reflns_number_total             1099
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hg5058.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 42/n c m'
_cod_database_code               2231141
_cod_database_fobs_code          2231141