An iron(III) complex salt containing pyrazole as both ligand and counter-ion: bis(1<i>H</i>-pyrazol-2-ium) pentacyanido(1<i>H</i>-pyrazole-κ<i>N</i>^2^)ferrate(III)
Wang, Yu-Feng; Yu, Chun-Hua; Zhu, Run-Qiang; Acta Crystallographica Section C 70 (2014) 437–439; doi:10.1107/S2053229614007128

data_2019469
_publ_section_title
;
 An iron(III) complex salt containing pyrazole as both ligand and
 counter-ion: bis(1<i>H</i>-pyrazol-2-ium)
 pentacyanido(1<i>H</i>-pyrazole-\k<i>N</i>^2^)ferrate(III)
;
_journal_coeditor_code           SF3226
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              437
_journal_page_last               439
_journal_paper_doi               10.1107/S2053229614007128
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '(C3 H5 N2)2 [Fe (C N)5 (C3 H4 N2)]'
_chemical_formula_moiety         '2(C3 H5 N2 +), C8 H4 Fe N7 2-'
_chemical_formula_sum            'C14 H14 Fe N11'
_chemical_formula_weight         392.21
_chemical_name_systematic
;
Bis(1<i>H</i>-pyrazol-2-ium)
pentacyanido(1<i>H</i>-pyrazole-\k<i>N</i>^2^)ferrate(III)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.19(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.0219(14)
_cell_length_b                   14.955(3)
_cell_length_c                   8.9722(18)
_cell_measurement_reflns_used    4324
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.21
_cell_volume                     942.0(3)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics
;
PLATON (Spek, 2009) and DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku SCXmini'
_diffrn_measurement_method       \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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9783
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 180
_diffrn_standards_interval_time  9
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.361
_refine_ls_abs_structure_details
'Flack (1983), <b>with how many Friedel pairs?</b>'
_refine_ls_abs_structure_Flack   0.009(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4324
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0227P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0710
_reflns_number_gt                4054
_reflns_number_total             4324
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3226sup1.cf
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2019469.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2019469
_cod_database_fobs_code          2019469