#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:46:34 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262575 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/19/7241904.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7241904
loop_
_publ_author_name
'Pérez, Hiram'
'Di Santo, Alejandro'
'Piro, Oscar E.'
'Echeverría, Gustavo A.'
'Cano, A.'
'González, M.'
'Rodríguez-Hernández, J.'
'Ben Altabef, A.'
'Frontera, Antonio'
'Gil, Diego M.'
_publ_section_title
;
 A first exploration of isostructurality in transition metal
 nitroprussides: X-ray analysis, magnetic properties and DFT calculations
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1158
_journal_page_last               1171
_journal_paper_doi               10.1039/D0CE01596B
_journal_volume                  23
_journal_year                    2021
_chemical_formula_sum            'C13 H12 Fe N10 O Zn'
_chemical_formula_weight         445.55
_chemical_name_systematic
catena-[tetrakis(u-cyano)-cyano-bis(1-methylimidazole)-nitrosyl-iron-zinc]
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-10-03 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8493(11)
_cell_length_b                   14.4980(10)
_cell_length_c                   16.5461(12)
_cell_measurement_reflns_used    1136
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      28.5230
_cell_measurement_theta_min      3.6480
_cell_volume                     3562.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      297(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0604
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.851
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_unetI/netI     0.1318
_diffrn_reflns_Laue_measured_fraction_full 0.851
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7971
_diffrn_reflns_point_group_measured_fraction_full 0.851
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_min         2.810
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1792
_exptl_crystal_recrystallization_method
'Crystals obtained employing a U-shaped tube by inter-diffusion of a sodium nitroprusside aqueous solution in one arm of the tube with a 1-methylimidazole solution of the metal chloride salt in the other arm.'
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.301
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.762
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         2946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.762
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0426P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1267
_reflns_number_total             2946
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01596b2.cif
_cod_data_source_block           shelx_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7241902--7241906.cif.'
_cod_database_code               7241904
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_cell_oxdiff_twin_number         2
_shelx_estimated_absorpt_t_min   0.776
_shelx_estimated_absorpt_t_max   0.882
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3376(5) 0.3812(4) 0.2447(3) 0.0162(14) Uani 1 1 d . . . . .
C2 C 0.3377(5) 0.1931(4) 0.2496(3) 0.0175(15) Uani 1 1 d . . . . .
C3 C 0.1527(5) 0.1950(4) 0.2141(3) 0.0185(16) Uani 1 1 d . . . . .
C4 C 0.1567(5) 0.3811(4) 0.2124(3) 0.0167(16) Uani 1 1 d . . . . .
C5 C 0.2728(5) 0.2822(4) 0.1239(3) 0.0205(16) Uani 1 1 d . . . . .
C11 C 0.5110(5) 0.4111(5) 0.0914(4) 0.037(2) Uani 1 1 d . . . . .
H11 H 0.4624 0.3747 0.1067 0.045 Uiso 1 1 calc R U . . .
C12 C 0.5621(5) 0.3973(5) 0.0252(4) 0.0310(19) Uani 1 1 d . . . . .
H12 H 0.5553 0.3503 -0.0126 0.037 Uiso 1 1 calc R U . . .
C13 C 0.6096(6) 0.5158(4) 0.0899(3) 0.0311(19) Uani 1 1 d . . . . .
H13 H 0.6445 0.5669 0.1032 0.037 Uiso 1 1 calc R U . . .
C14 C 0.6969(6) 0.4760(5) -0.0369(4) 0.049(2) Uani 1 1 d . . . . .
H14A H 0.7287 0.4189 -0.0439 0.074 Uiso 1 1 calc R U . . .
H14B H 0.7379 0.5226 -0.0185 0.074 Uiso 1 1 calc R U . . .
H14C H 0.6710 0.4946 -0.0875 0.074 Uiso 1 1 calc R U . . .
C21 C 0.3943(6) 0.5798(5) 0.4065(4) 0.041(2) Uani 1 1 d . . . . .
H21 H 0.3396 0.5600 0.3852 0.049 Uiso 1 1 calc R U . . .
C22 C 0.4045(7) 0.6124(6) 0.4812(4) 0.047(2) Uani 1 1 d . . . . .
H22 H 0.3598 0.6199 0.5200 0.056 Uiso 1 1 calc R U . . .
C23 C 0.5322(6) 0.6108(5) 0.4171(3) 0.035(2) Uani 1 1 d . . . . .
H23 H 0.5932 0.6179 0.4060 0.042 Uiso 1 1 calc R U . . .
C24 C 0.5399(6) 0.6683(5) 0.5596(3) 0.049(3) Uani 1 1 d . . . . .
H24A H 0.5827 0.7140 0.5428 0.073 Uiso 1 1 calc R U . . .
H24B H 0.5707 0.6189 0.5866 0.073 Uiso 1 1 calc R U . . .
H24C H 0.4971 0.6957 0.5959 0.073 Uiso 1 1 calc R U . . .
N N 0.2232(4) 0.2892(4) 0.3357(2) 0.0267(14) Uani 1 1 d . . . . .
N1 N 0.3920(4) 0.4354(4) 0.2500(2) 0.0244(14) Uani 1 1 d . . . . .
N2 N 0.3922(4) 0.1401(4) 0.2578(2) 0.0254(14) Uani 1 1 d . . . . .
N3 N 0.0988(4) 0.1415(4) 0.2045(3) 0.0254(14) Uani 1 1 d . . . . .
N4 N 0.1036(5) 0.4364(4) 0.2023(3) 0.0290(15) Uani 1 1 d . . . . .
N5 N 0.2939(4) 0.2795(4) 0.0575(3) 0.0395(17) Uani 1 1 d . . . . .
N11 N 0.5415(4) 0.4870(3) 0.1330(3) 0.0209(14) Uani 1 1 d . . . . .
N12 N 0.6237(4) 0.4633(4) 0.0243(2) 0.0269(14) Uani 1 1 d . . . . .
N21 N 0.4729(4) 0.5788(3) 0.3655(3) 0.0246(15) Uani 1 1 d . . . . .
N22 N 0.4929(5) 0.6322(4) 0.4890(3) 0.0341(16) Uani 1 1 d . . . . .
O O 0.2129(4) 0.2899(4) 0.4032(2) 0.066(2) Uani 1 1 d . . . . .
Fe Fe 0.24470(7) 0.28717(5) 0.23834(3) 0.0141(2) Uani 1 1 d . . . . .
Zn Zn 0.50110(7) 0.53730(4) 0.24679(4) 0.0181(2) Uani 1 1 d . . . . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Zn Zn 0.2839 1.4301 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 Fe 178.6(5) . . ?
N2 C2 Fe 178.3(6) . . ?
N3 C3 Fe 176.2(5) . . ?
N4 C4 Fe 175.5(5) . . ?
N5 C5 Fe 176.5(6) . . ?
C12 C11 N11 110.0(7) . . ?
N12 C12 C11 106.9(5) . . ?
N11 C13 N12 112.4(6) . . ?
C22 C21 N21 111.8(7) . . ?
C21 C22 N22 106.0(7) . . ?
N21 C23 N22 111.2(7) . . ?
O N Fe 176.6(5) . . ?
C1 N1 Zn 173.9(5) . . ?
C2 N2 Zn 171.1(4) . 3_645 ?
C3 N3 Zn 153.6(5) . 8_655 ?
C4 N4 Zn 149.8(4) . 6_556 ?
C13 N11 C11 103.7(5) . . ?
C13 N11 Zn 126.7(4) . . ?
C11 N11 Zn 129.1(5) . . ?
C12 N12 C13 107.1(6) . . ?
C12 N12 C14 126.8(5) . . ?
C13 N12 C14 126.2(6) . . ?
C23 N21 C21 104.5(5) . . ?
C23 N21 Zn 125.2(5) . . ?
C21 N21 Zn 130.3(5) . . ?
C23 N22 C22 106.5(6) . . ?
C23 N22 C24 125.2(8) . . ?
C22 N22 C24 128.2(6) . . ?
N Fe C2 93.2(2) . . ?
N Fe C1 94.2(2) . . ?
C2 Fe C1 89.0(3) . . ?
N Fe C3 94.5(3) . . ?
C2 Fe C3 92.1(3) . . ?
C1 Fe C3 171.2(2) . . ?
N Fe C4 94.3(2) . . ?
C2 Fe C4 172.5(2) . . ?
C1 Fe C4 89.9(2) . . ?
C3 Fe C4 87.9(2) . . ?
N Fe C5 178.4(3) . . ?
C2 Fe C5 85.2(2) . . ?
C1 Fe C5 85.8(2) . . ?
C3 Fe C5 85.7(2) . . ?
C4 Fe C5 87.4(2) . . ?
N21 Zn N11 173.6(2) . . ?
N21 Zn N2 88.94(19) . 3_655 ?
N11 Zn N2 89.93(19) . 3_655 ?
N21 Zn N1 91.33(19) . . ?
N11 Zn N1 89.92(19) . . ?
N2 Zn N1 178.9(2) 3_655 . ?
N21 Zn N3 88.06(19) . 8_665 ?
N11 Zn N3 98.26(18) . 8_665 ?
N2 Zn N3 90.5(2) 3_655 8_665 ?
N1 Zn N3 88.4(2) . 8_665 ?
N21 Zn N4 88.39(19) . 6_656 ?
N11 Zn N4 85.28(19) . 6_656 ?
N2 Zn N4 88.0(2) 3_655 6_656 ?
N1 Zn N4 93.0(2) . 6_656 ?
N3 Zn N4 176.19(18) 8_665 6_656 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.131(8) . ?
C1 Fe 1.942(7) . ?
C2 N2 1.125(8) . ?
C2 Fe 1.950(7) . ?
C3 N3 1.126(8) . ?
C3 Fe 1.953(7) . ?
C4 N4 1.137(7) . ?
C4 Fe 1.935(7) . ?
C5 N5 1.142(6) . ?
C5 Fe 1.941(5) . ?
C11 C12 1.347(9) . ?
C11 N11 1.374(7) . ?
C12 N12 1.324(8) . ?
C13 N11 1.307(8) . ?
C13 N12 1.343(7) . ?
C14 N12 1.496(9) . ?
C21 C22 1.331(9) . ?
C21 N21 1.351(9) . ?
C22 N22 1.350(10) . ?
C23 N21 1.312(8) . ?
C23 N22 1.362(8) . ?
C24 N22 1.458(8) . ?
N O 1.127(5) . ?
N Fe 1.643(4) . ?
N1 Zn 2.192(6) . ?
N2 Zn 2.176(6) 3_645 ?
N3 Zn 2.230(6) 8_655 ?
N4 Zn 2.273(6) 6_556 ?
N11 Zn 2.106(5) . ?
N21 Zn 2.096(5) . ?
Zn N2 2.176(6) 3_655 ?
Zn N3 2.230(6) 8_665 ?
Zn N4 2.273(6) 6_656 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C13 H13 N2 0.93 2.59 3.098(7) 114.8 3_655
C24 H24A N5 0.96 2.65 3.529(10) 152.6 3_655
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 1.0004 0.0012 0.0008 -0.0069 -0.9972 0.0328 0.0026 -0.0512 -0.9998
