#------------------------------------------------------------------------------
#$Date: 2020-08-07 06:26:32 +0300 (Fri, 07 Aug 2020) $
#$Revision: 255165 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/88/1558816.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_1558816
loop_
_publ_author_name
'Ibragimov, Avazbek'
_publ_section_title
;
 Bis(3,5-dinitrobenzoato-κO)bis(ethane-1,2-diamine-κ²N,N')cadmium(II)
;
_journal_coeditor_code           WM4132
_journal_issue                   7
_journal_name_full               IUCrData
_journal_page_first              x200843
_journal_paper_doi               10.1107/S2414314620008433
_journal_volume                  5
_journal_year                    2020
_chemical_formula_iupac          '[Cd (C7 H3 N2 O6)2 (C2 H8 N2)2)]'
_chemical_formula_moiety         'C18 H22 Cd N8 O12'
_chemical_formula_sum            'C18 H22 Cd N8 O12'
_chemical_formula_weight         654.83
_chemical_name_systematic
Bis(3,5-dinitrobenzoato-κO)bis(ethane-1,2-diamine-κ²N,N')cadmium(II)
_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   mixed
_atom_sites_solution_primary     Intrinsic-phasing
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                112.289(5)
_cell_angle_beta                 92.827(5)
_cell_angle_gamma                101.656(5)
_cell_formula_units_Z            1
_cell_length_a                   7.191(5)
_cell_length_b                   8.698(5)
_cell_length_c                   10.987(5)
_cell_measurement_reflns_used    3166
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      75.1240
_cell_measurement_theta_min      4.3670
_cell_volume                     616.7(6)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      291(2)
_diffrn_detector_area_resol_mean 10.2576
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4512
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.828
_diffrn_reflns_theta_min         4.392
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.810
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             330
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.506
_refine_ls_extinction_coef       0.0032(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018/3 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2482
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0327
_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)+(0.0513P)²+0.2183P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                2406
_reflns_number_total             2482
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm4132sup1.cif
_cod_data_source_block           I
_cod_database_code               1558816
_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   0.278
_shelx_estimated_absorpt_t_max   0.368
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
Cd Cd1 1.000000 0.500000 1.000000 0.04436(14) Uani d 1 . .
O O2 0.6549(4) 0.5433(4) 0.7930(3) 0.0651(7) Uani d 1 . .
O O1 0.8216(4) 0.3493(3) 0.7881(2) 0.0620(7) Uani d 1 . .
O O3 0.1233(4) 0.3373(4) 0.4291(3) 0.0715(8) Uani d 1 . .
O O4 0.1282(4) 0.1278(4) 0.2450(3) 0.0767(9) Uani d 1 . .
O O6 0.8565(4) -0.0927(4) 0.3594(3) 0.0730(8) Uani d 1 . .
N N1 0.1978(4) 0.2284(4) 0.3583(3) 0.0517(6) Uani d 1 . .
N N4 1.0222(4) 0.7651(3) 0.9904(3) 0.0487(6) Uani d 1 . .
O O5 0.6643(5) -0.1370(4) 0.1882(3) 0.0757(8) Uani d 1 . .
N N2 0.7258(4) -0.0609(4) 0.3057(3) 0.0516(6) Uani d 1 . .
C C2 0.6271(4) 0.3000(4) 0.5940(3) 0.0381(6) Uani d 1 . .
C C3 0.4603(4) 0.3208(4) 0.5398(3) 0.0396(6) Uani d 1 . .
H H3 0.402141 0.406126 0.589595 0.047 Uiso calc 1 . .
C C7 0.7155(4) 0.1743(4) 0.5164(3) 0.0395(6) Uani d 1 . .
H H7 0.827318 0.158989 0.551588 0.047 Uiso calc 1 . .
C C6 0.6340(4) 0.0733(4) 0.3869(3) 0.0397(6) Uani d 1 . .
C C4 0.3822(4) 0.2132(4) 0.4114(3) 0.0401(6) Uani d 1 . .
C C5 0.4662(4) 0.0883(4) 0.3320(3) 0.0426(6) Uani d 1 . .
H H5 0.411582 0.017367 0.245051 0.051 Uiso calc 1 . .
N N3 1.2449(5) 0.5152(5) 0.8698(4) 0.0714(10) Uani d 1 . .
C C1 0.7084(4) 0.4101(4) 0.7390(3) 0.0443(7) Uani d 1 . .
C C8 1.2033(6) 0.8097(5) 0.9427(4) 0.0622(9) Uani d 1 . .
H H8A 1.307671 0.851575 1.015179 0.075 Uiso calc 1 . .
H H8B 1.200122 0.900523 0.912486 0.075 Uiso calc 1 . .
C C9 1.2380(7) 0.6594(6) 0.8321(5) 0.0725(11) Uani d 1 . .
H H9A 1.136935 0.622053 0.758114 0.087 Uiso calc 1 . .
H H9B 1.358522 0.693491 0.802584 0.087 Uiso calc 1 . .
H H4A 0.922(4) 0.747(5) 0.928(3) 0.050(10) Uiso d 1 . .
H H4B 1.024(6) 0.846(4) 1.074(2) 0.072(13) Uiso d 1 . .
H H3A 1.336(4) 0.586(4) 0.940(3) 0.053(11) Uiso d 1 . .
H H3B 1.285(10) 0.419(8) 0.821(8) 0.27(6) Uiso 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 0.0181 0.0091 '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'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
N4 Cd1 N4 2_767 . 179.999(11) ?
N4 Cd1 N3 2_767 . 102.66(12) ?
N4 Cd1 N3 . . 77.34(12) ?
N4 Cd1 N3 2_767 2_767 77.34(12) ?
N4 Cd1 N3 . 2_767 102.66(12) ?
N3 Cd1 N3 . 2_767 180.0 ?
N4 Cd1 O1 2_767 . 86.36(10) ?
N4 Cd1 O1 . . 93.64(10) ?
N3 Cd1 O1 . . 80.38(15) ?
N3 Cd1 O1 2_767 . 99.63(15) ?
N4 Cd1 O1 2_767 2_767 93.64(10) ?
N4 Cd1 O1 . 2_767 86.36(10) ?
N3 Cd1 O1 . 2_767 99.62(15) ?
N3 Cd1 O1 2_767 2_767 80.37(15) ?
O1 Cd1 O1 . 2_767 180.00(8) ?
C1 O1 Cd1 . . 122.9(2) ?
O3 N1 O4 . . 124.1(3) ?
O3 N1 C4 . . 118.6(3) ?
O4 N1 C4 . . 117.3(3) ?
C8 N4 Cd1 . . 107.5(2) ?
C8 N4 H4A . . 109(2) ?
Cd1 N4 H4A . . 105(2) ?
C8 N4 H4B . . 109(3) ?
Cd1 N4 H4B . . 110(3) ?
H4A N4 H4B . . 117(4) ?
O5 N2 O6 . . 123.1(3) ?
O5 N2 C6 . . 118.1(3) ?
O6 N2 C6 . . 118.8(3) ?
C3 C2 C7 . . 119.7(3) ?
C3 C2 C1 . . 119.7(3) ?
C7 C2 C1 . . 120.5(3) ?
C4 C3 C2 . . 118.9(3) ?
C4 C3 H3 . . 120.5 ?
C2 C3 H3 . . 120.5 ?
C6 C7 C2 . . 118.8(3) ?
C6 C7 H7 . . 120.6 ?
C2 C7 H7 . . 120.6 ?
C5 C6 C7 . . 122.6(3) ?
C5 C6 N2 . . 118.6(3) ?
C7 C6 N2 . . 118.8(3) ?
C3 C4 C5 . . 122.8(3) ?
C3 C4 N1 . . 118.4(3) ?
C5 C4 N1 . . 118.8(3) ?
C6 C5 C4 . . 117.1(3) ?
C6 C5 H5 . . 121.5 ?
C4 C5 H5 . . 121.5 ?
C9 N3 Cd1 . . 106.2(2) ?
C9 N3 H3A . . 90(3) ?
Cd1 N3 H3A . . 95(3) ?
C9 N3 H3B . . 126(8) ?
Cd1 N3 H3B . . 121(7) ?
H3A N3 H3B . . 110(2) ?
O2 C1 O1 . . 128.6(3) ?
O2 C1 C2 . . 117.4(3) ?
O1 C1 C2 . . 114.0(3) ?
N4 C8 C9 . . 111.1(3) ?
N4 C8 H8A . . 109.4 ?
C9 C8 H8A . . 109.4 ?
N4 C8 H8B . . 109.4 ?
C9 C8 H8B . . 109.4 ?
H8A C8 H8B . . 108.0 ?
N3 C9 C8 . . 112.9(4) ?
N3 C9 H9A . . 109.0 ?
C8 C9 H9A . . 109.0 ?
N3 C9 H9B . . 109.0 ?
C8 C9 H9B . . 109.0 ?
H9A C9 H9B . . 107.8 ?
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
Cd1 N4 2_767 2.322(3) ?
Cd1 N4 . 2.322(3) ?
Cd1 N3 . 2.337(4) ?
Cd1 N3 2_767 2.337(4) ?
Cd1 O1 . 2.344(2) ?
Cd1 O1 2_767 2.344(2) ?
O2 C1 . 1.235(4) ?
O1 C1 . 1.257(4) ?
O3 N1 . 1.216(4) ?
O4 N1 . 1.226(4) ?
O6 N2 . 1.218(4) ?
N1 C4 . 1.473(4) ?
N4 C8 . 1.462(5) ?
N4 H4A . 0.916(10) ?
N4 H4B . 0.917(10) ?
O5 N2 . 1.216(4) ?
N2 C6 . 1.474(4) ?
C2 C3 . 1.388(4) ?
C2 C7 . 1.397(4) ?
C2 C1 . 1.524(4) ?
C3 C4 . 1.374(4) ?
C3 H3 . 0.9300 ?
C7 C6 . 1.379(4) ?
C7 H7 . 0.9300 ?
C6 C5 . 1.375(4) ?
C4 C5 . 1.380(4) ?
C5 H5 . 0.9300 ?
N3 C9 . 1.471(6) ?
N3 H3A . 0.914(10) ?
N3 H3B . 0.916(10) ?
C8 C9 . 1.485(6) ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
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
_geom_hbond_publ_flag
N4 H4A O2 . 0.916(10) 2.32(2) 3.099(4) 143(3) yes
N4 H4A O4 2_666 0.916(10) 2.56(3) 3.268(4) 134(3) yes
N4 H4B O4 1_666 0.917(10) 2.39(2) 3.237(4) 153(4) yes
N3 H3B O5 2_756 0.916(10) 2.52(7) 3.312(5) 145(10) yes
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
C7 C2 C3 C4 . . . . 1.8(4) ?
C1 C2 C3 C4 . . . . -175.9(3) ?
C3 C2 C7 C6 . . . . 0.0(4) ?
C1 C2 C7 C6 . . . . 177.8(3) ?
C2 C7 C6 C5 . . . . -1.8(4) ?
C2 C7 C6 N2 . . . . -179.2(3) ?
O5 N2 C6 C5 . . . . 9.9(4) ?
O6 N2 C6 C5 . . . . -168.6(3) ?
O5 N2 C6 C7 . . . . -172.6(3) ?
O6 N2 C6 C7 . . . . 8.9(4) ?
C2 C3 C4 C5 . . . . -2.2(4) ?
C2 C3 C4 N1 . . . . 175.6(3) ?
O3 N1 C4 C3 . . . . 1.3(5) ?
O4 N1 C4 C3 . . . . -177.9(3) ?
O3 N1 C4 C5 . . . . 179.2(3) ?
O4 N1 C4 C5 . . . . 0.0(4) ?
C7 C6 C5 C4 . . . . 1.5(4) ?
N2 C6 C5 C4 . . . . 178.9(3) ?
C3 C4 C5 C6 . . . . 0.5(4) ?
N1 C4 C5 C6 . . . . -177.3(3) ?
Cd1 O1 C1 O2 . . . . -8.4(5) ?
Cd1 O1 C1 C2 . . . . 172.57(19) ?
C3 C2 C1 O2 . . . . -19.2(4) ?
C7 C2 C1 O2 . . . . 163.0(3) ?
C3 C2 C1 O1 . . . . 159.9(3) ?
C7 C2 C1 O1 . . . . -17.8(4) ?
Cd1 N4 C8 C9 . . . . 42.2(4) ?
Cd1 N3 C9 C8 . . . . 41.0(5) ?
N4 C8 C9 N3 . . . . -59.1(5) ?

_cod_database_fobs_code 1558816
