#------------------------------------------------------------------------------
#$Date: 2022-07-23 06:53:46 +0300 (Sat, 23 Jul 2022) $
#$Revision: 276891 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/26/2022645.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_2022645
loop_
_publ_author_name
'Setifi, Zouaoui'
'Bernès, Sylvain'
'Geiger, David K.'
'Setifi, Fatima'
'Reedijk, Jan'
_publ_section_title
;
 Concomitant dimorphism in
 poly[di-μ-azido-(5,5'-dimethyl-2,2'-bipyridine)iron(II)]
;
_journal_coeditor_code           DG3032
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229622006908
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Fe (N3)2 (C12 H12 N2)]'
_chemical_formula_moiety         'C12 H12 Fe N8'
_chemical_formula_sum            'C12 H12 Fe N8'
_chemical_formula_weight         324.15
_chemical_name_systematic
catena-Poly[[(5,5'-dimethyl-2,2'-bipyridine-κ²N,N')iron(II)]-di-μ-azido-κ²N¹:N³-[(5,5'-dimethyl-2,2'-bipyridine-κ²N,N')iron(II)]-di-μ-azido-κ²N¹:N¹]
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                112.585(3)
_cell_angle_beta                 102.828(4)
_cell_angle_gamma                92.852(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7235(7)
_cell_length_b                   9.4051(7)
_cell_length_c                   10.5846(9)
_cell_measurement_reflns_used    9616
_cell_measurement_temperature    298.0(10)
_cell_measurement_theta_max      32.74
_cell_measurement_theta_min      2.37
_cell_volume                     684.36(10)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX2 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae et al.,
2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      298.0(10)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            54520
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.142
_diffrn_reflns_theta_min         2.372
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.9090
_exptl_absorpt_correction_T_min  0.8472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2017)
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       Prism
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.132
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.388
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     192
_refine_ls_number_reflns         5184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0368P)²+0.6298P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1281
_reflns_number_gt                3821
_reflns_number_total             5184
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            dg3032sup1.cif
_cod_data_source_block           I
_cod_database_code               2022645
_shelx_estimated_absorpt_t_min   0.674
_shelx_estimated_absorpt_t_max   0.868
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.31470(4) 0.39201(4) 0.49060(4) 0.03489(10) Uani d 1 . .
C C1 0.0681(3) 0.0841(3) 0.2645(3) 0.0426(5) Uani d 1 . .
H H1 0.036695 0.146193 0.215216 0.051 Uiso calc 1 . .
C C2 -0.0163(3) -0.0688(3) 0.2040(3) 0.0455(5) Uani d 1 . .
C C3 0.0307(4) -0.1575(3) 0.2817(3) 0.0498(6) Uani d 1 . .
H H3 -0.023499 -0.260461 0.246505 0.060 Uiso calc 1 . .
C C4 0.1573(4) -0.0938(3) 0.4105(3) 0.0451(5) Uani d 1 . .
H H4 0.188731 -0.153397 0.462327 0.054 Uiso calc 1 . .
C C5 0.2378(3) 0.0602(2) 0.4625(2) 0.0346(4) Uani d 1 . .
C C6 0.3736(3) 0.1392(2) 0.6000(2) 0.0341(4) Uani d 1 . .
C C7 0.4279(4) 0.0690(3) 0.6934(3) 0.0439(5) Uani d 1 . .
H H7 0.381975 -0.034011 0.669038 0.053 Uiso calc 1 . .
C C8 0.5500(4) 0.1528(3) 0.8220(3) 0.0459(5) Uani d 1 . .
H H8 0.585076 0.106822 0.885449 0.055 Uiso calc 1 . .
C C9 0.6205(3) 0.3055(3) 0.8572(3) 0.0411(5) Uani d 1 . .
C C10 0.5618(3) 0.3660(3) 0.7570(2) 0.0378(4) Uani d 1 . .
H H10 0.609093 0.467815 0.777970 0.045 Uiso calc 1 . .
C C11 -0.1515(4) -0.1316(4) 0.0621(3) 0.0621(8) Uani d 1 . .
H H11A -0.096083 -0.191935 -0.009813 0.093 Uiso calc 1 . .
H H11B -0.194391 -0.046578 0.041765 0.093 Uiso calc 1 . .
H H11C -0.250433 -0.196310 0.063597 0.093 Uiso calc 1 . .
C C12 0.7525(5) 0.4028(4) 0.9964(3) 0.0614(7) Uani d 1 . .
H H12A 0.689529 0.463788 1.062202 0.092 Uiso calc 1 . .
H H12B 0.836432 0.470794 0.982755 0.092 Uiso calc 1 . .
H H12C 0.815996 0.336070 1.033418 0.092 Uiso calc 1 . .
N N1 0.1920(2) 0.1485(2) 0.3892(2) 0.0356(4) Uani d 1 . .
N N2 0.4419(2) 0.2876(2) 0.6327(2) 0.0342(4) Uani d 1 . .
N N3 0.1346(3) 0.4453(3) 0.3358(2) 0.0483(5) Uani d 1 . .
N N4 0.0055(2) 0.5004(2) 0.35759(19) 0.0323(3) Uani d 1 . .
N N5 -0.1213(3) 0.5572(3) 0.3744(3) 0.0517(6) Uani d 1 . .
N N6 0.4691(3) 0.6197(2) 0.6137(2) 0.0401(4) Uani d 1 . .
N N7 0.4462(3) 0.7108(2) 0.7213(2) 0.0415(4) Uani d 1 . .
N N8 0.4226(5) 0.7980(3) 0.8239(3) 0.0795(10) Uani d 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3 Fe1 N6 . . 98.41(9) ?
N3 Fe1 N1 . . 91.43(9) ?
N6 Fe1 N1 . . 170.10(8) ?
N3 Fe1 N6 . 2_666 92.55(8) ?
N6 Fe1 N6 . 2_666 78.72(8) ?
N1 Fe1 N6 . 2_666 99.84(7) ?
N3 Fe1 N2 . . 164.94(8) ?
N6 Fe1 N2 . . 95.43(8) ?
N1 Fe1 N2 . . 74.91(7) ?
N6 Fe1 N2 2_666 . 95.97(7) ?
N3 Fe1 N5 . 2_566 90.37(8) ?
N6 Fe1 N5 . 2_566 91.51(9) ?
N1 Fe1 N5 . 2_566 89.53(9) ?
N6 Fe1 N5 2_666 2_566 170.11(9) ?
N2 Fe1 N5 . 2_566 83.33(7) ?
N1 C1 C2 . . 124.4(2) ?
N1 C1 H1 . . 117.8 ?
C2 C1 H1 . . 117.8 ?
C1 C2 C3 . . 116.4(2) ?
C1 C2 C11 . . 120.6(3) ?
C3 C2 C11 . . 123.0(3) ?
C4 C3 C2 . . 120.3(2) ?
C4 C3 H3 . . 119.8 ?
C2 C3 H3 . . 119.8 ?
C3 C4 C5 . . 119.6(2) ?
C3 C4 H4 . . 120.2 ?
C5 C4 H4 . . 120.2 ?
N1 C5 C4 . . 120.8(2) ?
N1 C5 C6 . . 115.63(19) ?
C4 C5 C6 . . 123.5(2) ?
N2 C6 C7 . . 120.8(2) ?
N2 C6 C5 . . 115.89(18) ?
C7 C6 C5 . . 123.3(2) ?
C8 C7 C6 . . 119.7(2) ?
C8 C7 H7 . . 120.2 ?
C6 C7 H7 . . 120.2 ?
C7 C8 C9 . . 120.1(2) ?
C7 C8 H8 . . 119.9 ?
C9 C8 H8 . . 119.9 ?
C8 C9 C10 . . 116.6(2) ?
C8 C9 C12 . . 122.4(2) ?
C10 C9 C12 . . 121.0(2) ?
N2 C10 C9 . . 124.2(2) ?
N2 C10 H10 . . 117.9 ?
C9 C10 H10 . . 117.9 ?
C2 C11 H11A . . 109.5 ?
C2 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C2 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C9 C12 H12A . . 109.5 ?
C9 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C9 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C1 N1 C5 . . 118.4(2) ?
C1 N1 Fe1 . . 124.67(16) ?
C5 N1 Fe1 . . 116.77(15) ?
C10 N2 C6 . . 118.59(19) ?
C10 N2 Fe1 . . 124.46(15) ?
C6 N2 Fe1 . . 116.22(15) ?
N4 N3 Fe1 . . 121.79(17) ?
N5 N4 N3 . . 176.9(2) ?
N4 N5 Fe1 . 2_566 143.68(18) ?
N7 N6 Fe1 . . 124.80(16) ?
N7 N6 Fe1 . 2_666 133.05(17) ?
Fe1 N6 Fe1 . 2_666 101.28(8) ?
N8 N7 N6 . . 179.4(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 N3 . 2.135(2) ?
Fe1 N6 . 2.149(2) ?
Fe1 N1 . 2.1770(19) ?
Fe1 N6 2_666 2.1825(19) ?
Fe1 N2 . 2.1832(18) ?
Fe1 N5 2_566 2.235(2) ?
C1 N1 . 1.338(3) ?
C1 C2 . 1.384(4) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.389(4) ?
C2 C11 . 1.502(4) ?
C3 C4 . 1.377(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.391(3) ?
C4 H4 . 0.9300 ?
C5 N1 . 1.349(3) ?
C5 C6 . 1.478(3) ?
C6 N2 . 1.350(3) ?
C6 C7 . 1.390(3) ?
C7 C8 . 1.377(4) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.385(4) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.390(3) ?
C9 C12 . 1.501(4) ?
C10 N2 . 1.333(3) ?
C10 H10 . 0.9300 ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
C12 H12A . 0.9600 ?
C12 H12B . 0.9600 ?
C12 H12C . 0.9600 ?
N3 N4 . 1.174(3) ?
N4 N5 . 1.154(3) ?
N6 N7 . 1.190(3) ?
N7 N8 . 1.142(3) ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C1 C2 C3 . . . . 1.3(4) ?
N1 C1 C2 C11 . . . . -178.9(2) ?
C1 C2 C3 C4 . . . . -1.0(4) ?
C11 C2 C3 C4 . . . . 179.2(3) ?
C2 C3 C4 C5 . . . . 0.1(4) ?
C3 C4 C5 N1 . . . . 0.8(4) ?
C3 C4 C5 C6 . . . . 179.4(2) ?
N1 C5 C6 N2 . . . . -3.1(3) ?
C4 C5 C6 N2 . . . . 178.2(2) ?
N1 C5 C6 C7 . . . . 175.7(2) ?
C4 C5 C6 C7 . . . . -3.0(3) ?
N2 C6 C7 C8 . . . . 1.4(4) ?
C5 C6 C7 C8 . . . . -177.4(2) ?
C6 C7 C8 C9 . . . . -1.1(4) ?
C7 C8 C9 C10 . . . . -0.1(4) ?
C7 C8 C9 C12 . . . . 179.4(3) ?
C8 C9 C10 N2 . . . . 1.0(4) ?
C12 C9 C10 N2 . . . . -178.4(2) ?
C2 C1 N1 C5 . . . . -0.6(4) ?
C2 C1 N1 Fe1 . . . . -176.49(18) ?
C4 C5 N1 C1 . . . . -0.5(3) ?
C6 C5 N1 C1 . . . . -179.29(19) ?
C4 C5 N1 Fe1 . . . . 175.71(17) ?
C6 C5 N1 Fe1 . . . . -3.1(2) ?
C9 C10 N2 C6 . . . . -0.8(3) ?
C9 C10 N2 Fe1 . . . . 169.09(17) ?
C7 C6 N2 C10 . . . . -0.5(3) ?
C5 C6 N2 C10 . . . . 178.38(19) ?
C7 C6 N2 Fe1 . . . . -171.17(17) ?
C5 C6 N2 Fe1 . . . . 7.7(2) ?

_cod_database_fobs_code 2022645
