#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/94/2019469.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2019469
loop_
_publ_author_name
'Wang, Yu-Feng'
'Yu, Chun-Hua'
'Zhu, Run-Qiang'
_publ_section_title
;
 An iron(III) complex salt containing pyrazole as both ligand and
 counter-ion: bis(1H-pyrazol-2-ium)
 pentacyanido(1H-pyrazole-κN²)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(1H-pyrazol-2-ium)
pentacyanido(1H-pyrazole-κN²)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       ω
_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), with how many Friedel pairs?'
_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/[σ²(Fo²)+(0.0227P)²+0.0000P] where P=(Fo²+2Fc²)/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>2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
C C1 0.9516(3) 0.95613(16) 0.8570(3) 0.0307(5) Uani d . 1 1
C C2 0.9554(3) 0.97455(15) 1.1628(3) 0.0310(5) Uani d . 1 1
C C3 0.6409(3) 1.08628(15) 1.1402(3) 0.0299(5) Uani d . 1 1
C C4 0.6405(3) 1.06832(15) 0.8337(3) 0.0310(5) Uani d . 1 1
C C5 0.9565(3) 1.12400(17) 0.9862(3) 0.0303(5) Uani d . 1 1
C C6 0.5295(4) 0.77643(18) 1.0404(3) 0.0450(7) Uani d . 1 1
H H6 0.5346 0.7146 1.0502 0.054 Uiso calc R 1 1
C C7 0.3672(4) 0.82821(17) 1.0342(3) 0.0464(7) Uani d . 1 1
H H7 0.2418 0.8086 1.0402 0.056 Uiso calc R 1 1
C C8 0.4288(3) 0.91463(17) 1.0174(3) 0.0343(5) Uani d . 1 1
H H8 0.3495 0.9643 1.0093 0.041 Uiso calc R 1 1
C C9 0.5215(4) 0.8659(2) 0.6366(3) 0.0534(7) Uani d . 1 1
H H9 0.5561 0.8472 0.7323 0.064 Uiso calc R 1 1
C C10 0.6429(4) 0.8772(2) 0.5213(3) 0.0516(7) Uani d . 1 1
H H10 0.7738 0.8677 0.5224 0.062 Uiso calc R 1 1
C C11 0.5324(4) 0.9053(2) 0.4051(3) 0.0543(8) Uani d . 1 1
H H11 0.5754 0.9194 0.3106 0.065 Uiso calc R 1 1
C C12 0.9262(5) 0.6552(3) 0.3973(3) 0.0739(11) Uani d . 1 1
H H12 0.9610 0.6497 0.2983 0.089 Uiso calc R 1 1
C C13 1.0434(5) 0.6787(3) 0.5125(4) 0.0762(10) Uani d . 1 1
H H13 1.1721 0.6930 0.5081 0.091 Uiso calc R 1 1
C C14 0.9350(4) 0.6773(2) 0.6350(3) 0.0591(8) Uani d . 1 1
H H14 0.9770 0.6903 0.7316 0.071 Uiso calc R 1 1
Fe Fe1 0.79424(4) 1.02011(2) 0.99859(3) 0.02194(8) Uani d . 1 1
N N1 1.0398(3) 0.91860(16) 0.7707(2) 0.0475(6) Uani d . 1 1
N N2 1.0465(3) 0.94890(17) 1.2607(2) 0.0521(6) Uani d . 1 1
N N3 0.5492(3) 1.12183(15) 1.2273(2) 0.0476(6) Uani d . 1 1
N N4 0.5522(3) 1.09499(16) 0.7347(2) 0.0504(6) Uani d . 1 1
N N5 1.0462(3) 1.18743(17) 0.9790(2) 0.0476(6) Uani d . 1 1
N N6 0.6206(3) 0.91734(11) 1.0142(2) 0.0251(4) Uani d . 1 1
N N7 0.6772(3) 0.83135(12) 1.0298(2) 0.0326(4) Uani d . 1 1
H H7A 0.7943 0.8144 1.0326 0.039 Uiso calc R 1 1
N N8 0.3536(3) 0.90949(16) 0.4477(2) 0.0491(6) Uani d . 1 1
H H8A 0.2577 0.9250 0.3924 0.059 Uiso calc R 1 1
N N9 0.3470(3) 0.88577(14) 0.5900(2) 0.0417(5) Uani d . 1 1
H H9A 0.2463 0.8837 0.6429 0.050 Uiso calc R 1 1
N N10 0.7598(3) 0.65436(15) 0.5955(2) 0.0436(5) Uani d . 1 1
H H10A 0.6656 0.6487 0.6545 0.052 Uiso calc R 1 1
N N11 0.7537(3) 0.64151(17) 0.4495(3) 0.0504(6) Uani d . 1 1
H H11A 0.6545 0.6267 0.3974 0.060 Uiso calc R 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N1 C1 Fe1 178.0(2) ?
N2 C2 Fe1 178.4(2) ?
N3 C3 Fe1 176.9(2) ?
N4 C4 Fe1 178.3(2) ?
N5 C5 Fe1 177.4(2) ?
N7 C6 C7 107.2(2) ?
N7 C6 H6 126.4 ?
C7 C6 H6 126.4 ?
C8 C7 C6 105.7(2) ?
C8 C7 H7 127.1 ?
C6 C7 H7 127.1 ?
N6 C8 C7 110.4(2) ?
N6 C8 H8 124.8 ?
C7 C8 H8 124.8 ?
N9 C9 C10 108.8(2) ?
N9 C9 H9 125.6 ?
C10 C9 H9 125.6 ?
C11 C10 C9 105.4(2) ?
C11 C10 H10 127.3 ?
C9 C10 H10 127.3 ?
N8 C11 C10 109.0(2) ?
N8 C11 H11 125.5 ?
C10 C11 H11 125.5 ?
N11 C12 C13 108.4(3) ?
N11 C12 H12 125.8 ?
C13 C12 H12 125.8 ?
C14 C13 C12 105.8(3) ?
C14 C13 H13 127.1 ?
C12 C13 H13 127.1 ?
N10 C14 C13 108.9(3) ?
N10 C14 H14 125.5 ?
C13 C14 H14 125.5 ?
C5 Fe1 C4 88.67(10) y
C5 Fe1 C1 90.82(10) y
C4 Fe1 C1 89.97(9) ?
C5 Fe1 C3 87.91(10) y
C4 Fe1 C3 90.11(9) ?
C1 Fe1 C3 178.72(11) ?
C5 Fe1 C2 89.48(10) y
C4 Fe1 C2 178.10(11) ?
C1 Fe1 C2 89.60(9) ?
C3 Fe1 C2 90.28(10) ?
C5 Fe1 N6 177.68(10) ?
C4 Fe1 N6 90.50(9) y
C1 Fe1 N6 91.35(9) y
C3 Fe1 N6 89.92(9) y
C2 Fe1 N6 91.36(9) y
C8 N6 N7 105.13(18) ?
C8 N6 Fe1 130.19(15) ?
N7 N6 Fe1 124.64(14) ?
C6 N7 N6 111.5(2) ?
C6 N7 H7A 124.2 ?
N6 N7 H7A 124.2 ?
C11 N8 N9 108.5(2) ?
C11 N8 H8A 125.7 ?
N9 N8 H8A 125.7 ?
C9 N9 N8 108.3(2) ?
C9 N9 H9A 125.9 ?
N8 N9 H9A 125.9 ?
C14 N10 N11 108.3(2) ?
C14 N10 H10A 125.8 ?
N11 N10 H10A 125.8 ?
C12 N11 N10 108.5(2) ?
C12 N11 H11A 125.8 ?
N10 N11 H11A 125.8 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 1.148(3) ?
C1 Fe1 1.951(2) y
C2 N2 1.142(3) ?
C2 Fe1 1.961(2) y
C3 N3 1.153(3) ?
C3 Fe1 1.952(2) y
C4 N4 1.145(3) ?
C4 Fe1 1.951(2) y
C5 N5 1.141(3) ?
C5 Fe1 1.931(3) y
C6 N7 1.328(3) ?
C6 C7 1.378(4) ?
C6 H6 0.9300 ?
C7 C8 1.372(3) ?
C7 H7 0.9300 ?
C8 N6 1.348(3) ?
C8 H8 0.9300 ?
C9 N9 1.321(3) ?
C9 C10 1.364(4) ?
C9 H9 0.9300 ?
C10 C11 1.353(4) ?
C10 H10 0.9300 ?
C11 N8 1.322(3) ?
C11 H11 0.9300 ?
C12 N11 1.324(4) ?
C12 C13 1.354(4) ?
C12 H12 0.9300 ?
C13 C14 1.350(4) ?
C13 H13 0.9300 ?
C14 N10 1.318(3) ?
C14 H14 0.9300 ?
Fe1 N6 1.9686(18) y
N6 N7 1.352(2) ?
N7 H7A 0.8600 ?
N8 N9 1.327(3) ?
N8 H8A 0.8600 ?
N9 H9A 0.8600 ?
N10 N11 1.324(3) ?
N10 H10A 0.8600 ?
N11 H11A 0.8600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N7 H7A N5 2_747 0.86 2.21 2.901(3) 137.6
N8 H8A N2 1_454 0.86 1.91 2.768(3) 174.7
N9 H9A N1 1_455 0.86 1.94 2.769(3) 161.8
N10 H10A N3 2_647 0.86 1.90 2.760(3) 172.6
N11 H11A N4 2_646 0.86 1.91 2.771(3) 174.7
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N7 C6 C7 C8 0.9(3)
C6 C7 C8 N6 -0.4(3)
N9 C9 C10 C11 0.4(4)
C9 C10 C11 N8 -0.8(4)
N11 C12 C13 C14 0.8(5)
C12 C13 C14 N10 -0.3(4)
N5 C5 Fe1 C4 51(5)
N5 C5 Fe1 C1 140(5)
N5 C5 Fe1 C3 -40(5)
N5 C5 Fe1 C2 -130(5)
N5 C5 Fe1 N6 -19(7)
N4 C4 Fe1 C5 106(8)
N4 C4 Fe1 C1 16(8)
N4 C4 Fe1 C3 -166(8)
N4 C4 Fe1 C2 92(9)
N4 C4 Fe1 N6 -76(8)
N1 C1 Fe1 C5 -112(6)
N1 C1 Fe1 C4 -23(6)
N1 C1 Fe1 C3 -117(7)
N1 C1 Fe1 C2 159(6)
N1 C1 Fe1 N6 67(6)
N3 C3 Fe1 C5 -143(4)
N3 C3 Fe1 C4 128(4)
N3 C3 Fe1 C1 -138(5)
N3 C3 Fe1 C2 -53(4)
N3 C3 Fe1 N6 38(4)
N2 C2 Fe1 C5 94(9)
N2 C2 Fe1 C4 108(9)
N2 C2 Fe1 C1 -18E1(10)
N2 C2 Fe1 C3 6(9)
N2 C2 Fe1 N6 -84(9)
C7 C8 N6 N7 -0.2(3)
C7 C8 N6 Fe1 -178.04(18)
C5 Fe1 N6 C8 21(2)
C4 Fe1 N6 C8 -47.5(2)
C1 Fe1 N6 C8 -137.5(2)
C3 Fe1 N6 C8 42.6(2)
C2 Fe1 N6 C8 132.9(2)
C5 Fe1 N6 N7 -156(2)
C4 Fe1 N6 N7 135.01(18)
C1 Fe1 N6 N7 45.02(18)
C3 Fe1 N6 N7 -134.88(18)
C2 Fe1 N6 N7 -44.60(18)
C7 C6 N7 N6 -1.1(3)
C8 N6 N7 C6 0.8(3)
Fe1 N6 N7 C6 178.79(16)
C10 C11 N8 N9 0.8(4)
C10 C9 N9 N8 0.1(4)
C11 N8 N9 C9 -0.6(3)
C13 C14 N10 N11 -0.3(4)
C13 C12 N11 N10 -1.0(4)
C14 N10 N11 C12 0.8(3)
