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#$Date: 2021-07-05 20:05:48 +0200 (lun 05 de jul de 2021) $
#$Revision: 267220 $
#$URL: svn://www.crystallography.net/cod/cif/7/06/06/7060640.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_7060640
loop_
_publ_author_name
'Braun, Vanessa'
'Wurzenberger, Maximilian H. H.'
'Weippert, Valentin'
'Stierstorfer, Jörg'
_publ_section_title
;
 Tailoring the properties of 3d transition metal complexes with different
 N-cycloalkyl-substituted tetrazoles
;
_journal_issue                   25
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11042
_journal_page_last               11050
_journal_paper_doi               10.1039/D1NJ01675J
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         '	C24 H36 Fe N24, 2(Cl O4)'
_chemical_formula_sum            'C24 H36 Cl2 Fe N24 O8'
_chemical_formula_weight         915.52
_chemical_name_common
'hexakis(1-cyclopropyl-5H-tetrazolyl)iron(II) diperchlorate'
_chemical_name_systematic
'hexakis(1-cyclopropyl-5H-tetrazolyl)iron(II) diperchlorate'
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-02-04 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.83930(10)
_cell_length_b                   10.83930(10)
_cell_length_c                   30.1945(6)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      30.4238
_cell_measurement_theta_min      3.4633
_cell_volume                     3072.28(7)
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            19341
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.343
_diffrn_reflns_theta_min         2.555
_diffrn_source                   'rotating anode generator'
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.195
_refine_ls_extinction_coef       0.043(4)
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1096P)²+5.1691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.1712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1328
_reflns_number_total             1401
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj01675j2.cif
_cod_data_source_block           yv333
_cod_depositor_comments
'Adding full bibliography for 7060620--7060640.cif.'
_cod_original_cell_volume        3072.28(8)
_cod_original_sg_symbol_H-M      'R -3 '
_cod_database_code               7060640
_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.
;
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.894
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Fe1 Fe 1.000000 1.000000 0.500000 0.0288(4) Uani 1 6 d S T P . .
Cl1 Cl 0.333333 0.666667 0.51062(4) 0.0470(4) Uani 1 3 d S T P . .
N4 N 0.7213(2) 0.6405(2) 0.58097(7) 0.0377(6) Uani 1 1 d . . . . .
N1 N 0.8780(2) 0.8127(2) 0.54200(7) 0.0365(6) Uani 1 1 d . . . . .
N3 N 0.8493(3) 0.6714(3) 0.59657(10) 0.0587(8) Uani 1 1 d . . . . .
C1 C 0.7416(3) 0.7270(3) 0.54745(9) 0.0401(6) Uani 1 1 d . . . . .
N2 N 0.9432(3) 0.7752(3) 0.57328(10) 0.0559(8) Uani 1 1 d . . . . .
C2 C 0.5912(3) 0.5191(3) 0.59677(10) 0.0468(7) Uani 1 1 d . . . . .
C4 C 0.4857(4) 0.5440(5) 0.61983(14) 0.0655(10) Uani 1 1 d . . . . .
C3 C 0.5703(4) 0.4970(4) 0.64513(10) 0.0575(9) Uani 1 1 d . . . . .
H3A H 0.522482 0.399809 0.656012 0.069 Uiso 1 1 calc R U . . .
H3B H 0.644501 0.565943 0.664363 0.069 Uiso 1 1 calc R U . . .
O1 O 0.2358(5) 0.5301(4) 0.49415(17) 0.1250(17) Uani 1 1 d . . . . .
O2 O 0.333333 0.666667 0.5559(2) 0.160(4) Uani 1 3 d S T P . .
H1 H 0.676(4) 0.723(4) 0.5339(13) 0.051(9) Uiso 1 1 d . . . . .
H4A H 0.513(5) 0.624(6) 0.6205(16) 0.072(14) Uiso 1 1 d . . . . .
H2 H 0.570(5) 0.439(5) 0.5783(15) 0.069(12) Uiso 1 1 d . . . . .
H4B H 0.390(5) 0.472(5) 0.6107(15) 0.074(12) Uiso 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'
Cl Cl 0.1484 0.1585 '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'
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 Fe1 N1 90.18(8) . 11_566 ?
N1 Fe1 N1 89.82(8) . 2_765 ?
N1 Fe1 N1 180.0 11_566 2_765 ?
N1 Fe1 N1 90.18(8) . 12_656 ?
N1 Fe1 N1 89.82(8) 11_566 12_656 ?
N1 Fe1 N1 90.18(8) 2_765 12_656 ?
N1 Fe1 N1 89.82(8) . 3_675 ?
N1 Fe1 N1 90.18(8) 11_566 3_675 ?
N1 Fe1 N1 89.82(8) 2_765 3_675 ?
N1 Fe1 N1 180.00(9) 12_656 3_675 ?
N1 Fe1 N1 180.0 . 10_776 ?
N1 Fe1 N1 89.82(8) 11_566 10_776 ?
N1 Fe1 N1 90.18(8) 2_765 10_776 ?
N1 Fe1 N1 89.82(8) 12_656 10_776 ?
N1 Fe1 N1 90.18(8) 3_675 10_776 ?
O2 Cl1 O1 110.6(2) . 3_565 ?
O2 Cl1 O1 110.6(2) . . ?
O1 Cl1 O1 108.3(2) 3_565 . ?
O2 Cl1 O1 110.6(2) . 2_665 ?
O1 Cl1 O1 108.3(2) 3_565 2_665 ?
O1 Cl1 O1 108.3(2) . 2_665 ?
C1 N4 N3 107.9(2) . . ?
C1 N4 C2 129.7(2) . . ?
N3 N4 C2 121.9(2) . . ?
C1 N1 N2 105.9(2) . . ?
C1 N1 Fe1 132.60(18) . . ?
N2 N1 Fe1 121.14(16) . . ?
N2 N3 N4 107.1(2) . . ?
N1 C1 N4 109.2(2) . . ?
N1 C1 H1 129(3) . . ?
N4 C1 H1 122(3) . . ?
N3 N2 N1 109.9(2) . . ?
N4 C2 C4 118.8(3) . . ?
N4 C2 C3 118.3(3) . . ?
C4 C2 C3 59.6(3) . . ?
N4 C2 H2 108(3) . . ?
C4 C2 H2 126(3) . . ?
C3 C2 H2 119(3) . . ?
C3 C4 C2 60.4(2) . . ?
C3 C4 H4A 115(4) . . ?
C2 C4 H4A 109(4) . . ?
C3 C4 H4B 118(3) . . ?
C2 C4 H4B 110(3) . . ?
H4A C4 H4B 125(5) . . ?
C4 C3 C2 60.1(2) . . ?
C4 C3 H3A 117.8 . . ?
C2 C3 H3A 117.8 . . ?
C4 C3 H3B 117.8 . . ?
C2 C3 H3B 117.8 . . ?
H3A C3 H3B 114.9 . . ?
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
Fe1 N1 2.190(2) . ?
Fe1 N1 2.190(2) 11_566 ?
Fe1 N1 2.190(2) 2_765 ?
Fe1 N1 2.190(2) 12_656 ?
Fe1 N1 2.190(2) 3_675 ?
Fe1 N1 2.190(2) 10_776 ?
Cl1 O2 1.368(6) . ?
Cl1 O1 1.411(4) 3_565 ?
Cl1 O1 1.411(4) . ?
Cl1 O1 1.411(4) 2_665 ?
N4 C1 1.321(3) . ?
N4 N3 1.340(3) . ?
N4 C2 1.447(3) . ?
N1 C1 1.305(3) . ?
N1 N2 1.357(3) . ?
N3 N2 1.285(4) . ?
C1 H1 0.81(4) . ?
C2 C4 1.474(5) . ?
C2 C3 1.479(4) . ?
C2 H2 0.96(4) . ?
C4 C3 1.467(6) . ?
C4 H4A 0.76(5) . ?
C4 H4B 0.98(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
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
? ? ? ? ? ? ? ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N4 N3 N2 0.9(4) . . . . ?
C2 N4 N3 N2 173.8(3) . . . . ?
N2 N1 C1 N4 0.7(3) . . . . ?
Fe1 N1 C1 N4 -171.89(18) . . . . ?
N3 N4 C1 N1 -1.0(3) . . . . ?
C2 N4 C1 N1 -173.1(3) . . . . ?
N4 N3 N2 N1 -0.5(4) . . . . ?
C1 N1 N2 N3 -0.1(4) . . . . ?
Fe1 N1 N2 N3 173.5(2) . . . . ?
C1 N4 C2 C4 -72.1(4) . . . . ?
N3 N4 C2 C4 116.7(4) . . . . ?
C1 N4 C2 C3 -141.0(3) . . . . ?
N3 N4 C2 C3 47.8(4) . . . . ?
N4 C2 C4 C3 -107.7(3) . . . . ?
N4 C2 C3 C4 108.6(4) . . . . ?
