#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/67/2216719.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_2216719
loop_
_publ_author_name
'Chundak, S. Yu.'
'Lukachinec, L. Yu.'
'Daszkiewicz, M.'
_publ_section_title
;Di-μ-nitrato-κ³O,O':O'';κ³O:O',O''-bis[bis(3-nitrobenzohydrazide-κ²N',O)cadmium(II)]
 dinitrate
;
_journal_coeditor_code           PV2040
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2893
_journal_page_last               m2893
_journal_paper_doi               10.1107/S1600536807053792
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cd2 (N O3)2 (C7 H7 N3 O3)2 ](N O3)2'
_chemical_formula_moiety         'C14 H14 Cd N7 O9, N O3'
_chemical_formula_sum            'C14 H14 Cd N8 O12'
_chemical_formula_weight         598.73
_chemical_name_systematic
;
Di-μ-nitrato-κ³O,O':O'';κ³O:O',O''-bis[bis(3-nitrobenzohydrazide-
κ²N',O)cadmium(II)] dinitrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.67(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9218(16)
_cell_length_b                   7.6237(15)
_cell_length_c                   34.325(7)
_cell_measurement_reflns_used    3275
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      3.21
_cell_volume                     2068.8(7)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'publCIF (Version 1.9.0_c; Westrip, 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2, 33.133pixel/mm'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Kuma KM-4 with CCD area-detector'
_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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            26291
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  0.8707
_exptl_absorpt_correction_T_min  0.6723
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(CrysAlis; Oxford Diffraction, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.763
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5111
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0409
_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)+(0.0233P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                3275
_reflns_number_total             5111
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pv2040.cif
_cod_data_source_block           I
_cod_original_cell_volume        2068.7(7)
_cod_database_code               2216719
_cod_database_fobs_code          2216719
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Cd Cd1 0.21123(3) 0.91697(3) 0.065750(7) 0.03871(9) Uani d . 1
C C1A 0.3993(3) 1.3516(4) 0.14429(8) 0.0283(7) Uani d . 1
C C11A 0.3681(4) 1.2144(4) 0.11357(8) 0.0299(7) Uani d . 1
O O11A 0.2649(3) 1.0959(3) 0.11856(6) 0.0420(5) Uani d . 1
N N11A 0.4532(3) 1.2260(3) 0.08142(7) 0.0325(6) Uani d . 1
H H11A 0.5254 1.3101 0.0774 0.049 Uiso d . 1
N N12A 0.4232(3) 1.0998(3) 0.05130(7) 0.0348(6) Uani d . 1
H H21A 0.3816 1.1528 0.0296 0.052 Uiso d . 1
H H22A 0.5221 1.0456 0.0503 0.052 Uiso d . 1
C C2A 0.4693(3) 1.5141(4) 0.13664(9) 0.0305(7) Uani d . 1
H H2A 0.5050 1.5402 0.1120 0.037 Uiso calc R 1
C C3A 0.4847(4) 1.6360(4) 0.16640(9) 0.0320(7) Uani d . 1
N N31A 0.5536(4) 1.8102(4) 0.15805(9) 0.0488(7) Uani d . 1
O O31A 0.5797(4) 1.8452(3) 0.12432(8) 0.0784(9) Uani d . 1
O O32A 0.5794(4) 1.9129(3) 0.18495(8) 0.0781(8) Uani d . 1
C C4A 0.4352(4) 1.6029(4) 0.20352(9) 0.0406(8) Uani d . 1
H H4A 0.4474 1.6873 0.2231 0.049 Uiso calc R 1
C C5A 0.3668(4) 1.4395(4) 0.21075(9) 0.0431(8) Uani d . 1
H H5A 0.3332 1.4133 0.2356 0.052 Uiso calc R 1
C C6A 0.3481(3) 1.3157(4) 0.18157(8) 0.0351(8) Uani d . 1
H H6A 0.3009 1.2072 0.1868 0.042 Uiso calc R 1
C C1B -0.0259(3) 0.4933(4) 0.13333(8) 0.0280(7) Uani d . 1
C C11B 0.0584(3) 0.6052(4) 0.10467(8) 0.0292(7) Uani d . 1
O O11B 0.1456(3) 0.7319(3) 0.11554(6) 0.0422(6) Uani d . 1
N N11B 0.0386(3) 0.5559(3) 0.06711(7) 0.0345(6) Uani d . 1
H H11B -0.0480 0.4930 0.0575 0.052 Uiso d . 1
N N12B 0.1088(3) 0.6642(3) 0.03862(7) 0.0342(6) Uani d . 1
H H21B 0.0277 0.6993 0.0207 0.051 Uiso d . 1
H H22B 0.1590 0.5965 0.0233 0.051 Uiso d . 1
C C2B -0.0491(3) 0.5612(4) 0.16999(9) 0.0345(7) Uani d . 1
H H2B -0.0152 0.6750 0.1764 0.041 Uiso calc R 1
C C3B -0.1232(4) 0.4572(4) 0.19677(9) 0.0383(8) Uani d . 1
N N31B -0.1504(4) 0.5325(5) 0.23589(9) 0.0575(9) Uani d . 1
O O31B -0.1058(4) 0.6833(5) 0.24205(8) 0.0936(10) Uani d . 1
O O32B -0.2169(4) 0.4419(4) 0.25973(8) 0.0890(10) Uani d . 1
C C4B -0.1743(4) 0.2890(5) 0.18912(10) 0.0467(9) Uani d . 1
H H4B -0.2244 0.2222 0.2079 0.056 Uiso calc R 1
C C5B -0.1495(4) 0.2211(4) 0.15282(10) 0.0461(9) Uani d . 1
H H5B -0.1831 0.1067 0.1469 0.055 Uiso calc R 1
C C6B -0.0751(4) 0.3213(4) 0.12507(9) 0.0365(8) Uani d . 1
H H6B -0.0578 0.2735 0.1007 0.044 Uiso calc R 1
N N1A -0.1265(3) 1.0524(3) 0.03837(8) 0.0355(6) Uani d . 1
O O1A 0.0176(3) 1.1213(3) 0.03396(6) 0.0446(6) Uani d . 1
O O2A -0.1387(3) 0.9443(3) 0.06509(7) 0.0578(7) Uani d . 1
O O3A -0.2493(3) 1.0939(3) 0.01617(6) 0.0458(6) Uani d . 1
N N1B 0.6356(3) 0.5968(4) 0.03179(7) 0.0369(6) Uani d . 1
O O1B 0.6860(3) 0.4722(3) 0.05402(6) 0.0470(6) Uani d . 1
O O2B 0.7298(3) 0.6450(3) 0.00571(6) 0.0483(6) Uani d . 1
O O3B 0.4979(3) 0.6670(3) 0.03588(7) 0.0605(7) 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'
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'
Cd Cd -0.8075 1.2024 '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
N12A Cd1 N12B 133.23(9) y
N12A Cd1 O11A 72.73(8) y
N12A Cd1 O11B 138.33(8) y
N12A Cd1 O1A 87.82(8) y
N12B Cd1 O11B 72.07(8) y
N12B Cd1 O11A 151.16(8) y
N12B Cd1 O1A 99.40(8) y
O11A Cd1 O11B 79.41(7) y
O11A Cd1 O1A 93.12(8) y
O11B Cd1 O1A 124.58(8) y
C2A C1A C6A 119.5(3) ?
C2A C1A C11A 122.7(3) ?
C6A C1A C11A 117.8(3) ?
O11A C11A N11A 122.5(3) ?
O11A C11A C1A 119.6(3) ?
N11A C11A C1A 117.9(3) ?
C11A O11A Cd1 114.63(18) ?
C11A N11A N12A 119.2(2) ?
C11A N11A H11A 123.3 ?
N12A N11A H11A 117.5 ?
N11A N12A Cd1 110.48(16) ?
N11A N12A H21A 109.7 ?
Cd1 N12A H21A 102.8 ?
N11A N12A H22A 103.7 ?
Cd1 N12A H22A 113.0 ?
H21A N12A H22A 117.3 ?
C3A C2A C1A 118.5(3) ?
C3A C2A H2A 120.7 ?
C1A C2A H2A 120.7 ?
C4A C3A C2A 122.9(3) ?
C4A C3A N31A 118.4(3) ?
C2A C3A N31A 118.7(3) ?
O32A N31A O31A 123.3(3) ?
O32A N31A C3A 118.6(3) ?
O31A N31A C3A 118.1(3) ?
C3A C4A C5A 117.8(3) ?
C3A C4A H4A 121.1 ?
C5A C4A H4A 121.1 ?
C6A C5A C4A 120.7(3) ?
C6A C5A H5A 119.7 ?
C4A C5A H5A 119.7 ?
C5A C6A C1A 120.6(3) ?
C5A C6A H6A 119.7 ?
C1A C6A H6A 119.7 ?
C2B C1B C6B 119.1(3) ?
C2B C1B C11B 118.4(3) ?
C6B C1B C11B 122.4(3) ?
O11B C11B N11B 122.6(3) ?
O11B C11B C1B 121.0(3) ?
N11B C11B C1B 116.3(3) ?
C11B O11B Cd1 113.88(18) ?
C11B N11B N12B 118.2(2) ?
C11B N11B H11B 123.3 ?
N12B N11B H11B 112.9 ?
N11B N12B Cd1 110.89(16) ?
N11B N12B H21B 110.5 ?
Cd1 N12B H21B 104.4 ?
N11B N12B H22B 107.0 ?
Cd1 N12B H22B 126.8 ?
H21B N12B H22B 95.6 ?
C3B C2B C1B 118.6(3) ?
C3B C2B H2B 120.7 ?
C1B C2B H2B 120.7 ?
C4B C3B C2B 123.2(3) ?
C4B C3B N31B 118.5(3) ?
C2B C3B N31B 118.2(3) ?
O32B N31B O31B 123.6(4) ?
O32B N31B C3B 118.8(3) ?
O31B N31B C3B 117.7(3) ?
C3B C4B C5B 118.0(3) ?
C3B C4B H4B 121.0 ?
C5B C4B H4B 121.0 ?
C4B C5B C6B 120.6(3) ?
C4B C5B H5B 119.7 ?
C6B C5B H5B 119.7 ?
C5B C6B C1B 120.4(3) ?
C5B C6B H6B 119.8 ?
C1B C6B H6B 119.8 ?
O3A N1A O2A 122.0(3) ?
O3A N1A O1A 119.8(3) ?
O2A N1A O1A 118.3(3) ?
N1A O1A Cd1 103.30(18) ?
O3B N1B O2B 121.6(3) ?
O3B N1B O1B 120.3(3) ?
O2B N1B O1B 118.0(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
Cd1 O11A . 2.287(2) y
Cd1 O11B . 2.301(2) y
Cd1 N12A . 2.262(2) y
Cd1 N12B . 2.268(2) y
Cd1 O1A . 2.399(2) y
Cd1 O2A . 2.778(2) y
Cd1 O3A 3_575 2.848(2) y
Cd1 O3B . 3.184(3) y
C1A C2A . 1.389(4) ?
C1A C6A . 1.394(4) ?
C1A C11A . 1.494(4) ?
C11A O11A . 1.238(3) ?
C11A N11A . 1.333(3) ?
N11A N12A . 1.421(3) ?
N11A H11A . 0.8760 ?
N12A H21A . 0.8908 ?
N12A H22A . 0.8890 ?
C2A C3A . 1.381(4) ?
C2A H2A . 0.9300 ?
C3A C4A . 1.380(4) ?
C3A N31A . 1.471(4) ?
N31A O32A . 1.218(3) ?
N31A O31A . 1.219(3) ?
C4A C5A . 1.387(4) ?
C4A H4A . 0.9300 ?
C5A C6A . 1.377(4) ?
C5A H5A . 0.9300 ?
C6A H6A . 0.9300 ?
C1B C2B . 1.384(4) ?
C1B C6B . 1.392(4) ?
C1B C11B . 1.492(4) ?
C11B O11B . 1.232(3) ?
C11B N11B . 1.342(3) ?
N11B N12B . 1.420(3) ?
N11B H11B . 0.8831 ?
N12B H21B . 0.9017 ?
N12B H22B . 0.8532 ?
C2B C3B . 1.374(4) ?
C2B H2B . 0.9300 ?
C3B C4B . 1.365(4) ?
C3B N31B . 1.489(4) ?
N31B O32B . 1.216(4) ?
N31B O31B . 1.217(4) ?
C4B C5B . 1.375(4) ?
C4B H4B . 0.9300 ?
C5B C6B . 1.382(4) ?
C5B H5B . 0.9300 ?
C6B H6B . 0.9300 ?
N1A O3A . 1.238(3) ?
N1A O2A . 1.241(3) ?
N1A O1A . 1.274(3) ?
N1B O3B . 1.232(3) ?
N1B O2B . 1.256(3) ?
N1B O1B . 1.267(3) ?
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
N11A H11A O1B 1_565 0.88 1.98 2.833(3) 164.5
N12A H21A O2B 3_675 0.89 2.12 2.963(3) 157.8
N12A H22A O3A 1_655 0.89 2.25 2.931(3) 133.3
N11B H11B O1B 1_455 0.88 2.11 2.872(3) 144.3
N12B H21B O1A 3_575 0.90 2.33 3.093(3) 142.2
N12B H21B O2B 1_455 0.90 2.42 3.143(3) 137.5
N12B H22B O2B 3_665 0.85 2.30 3.124(3) 163.6
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
C2A C1A C11A O11A -159.5(3)
C6A C1A C11A O11A 17.5(4)
C2A C1A C11A N11A 20.1(4)
C6A C1A C11A N11A -162.9(3)
N11A C11A O11A Cd1 -6.3(4)
C1A C11A O11A Cd1 173.26(19)
N12A Cd1 O11A C11A 6.32(19)
N12B Cd1 O11A C11A 163.6(2)
O11B Cd1 O11A C11A 155.0(2)
O1A Cd1 O11A C11A -80.4(2)
O11A C11A N11A N12A 1.1(4)
C1A C11A N11A N12A -178.5(2)
C11A N11A N12A Cd1 4.7(3)
N12B Cd1 N12A N11A -170.52(15)
O11A Cd1 N12A N11A -5.34(16)
O11B Cd1 N12A N11A -55.6(2)
O1A Cd1 N12A N11A 88.61(17)
C6A C1A C2A C3A -0.5(4)
C11A C1A C2A C3A 176.5(3)
C1A C2A C3A C4A 0.7(4)
C1A C2A C3A N31A -178.1(3)
C4A C3A N31A O32A 6.8(4)
C2A C3A N31A O32A -174.4(3)
C4A C3A N31A O31A -172.1(3)
C2A C3A N31A O31A 6.7(4)
C2A C3A C4A C5A -0.2(5)
N31A C3A C4A C5A 178.5(3)
C3A C4A C5A C6A -0.5(5)
C4A C5A C6A C1A 0.7(5)
C2A C1A C6A C5A -0.2(4)
C11A C1A C6A C5A -177.3(3)
C2B C1B C11B O11B 19.6(4)
C6B C1B C11B O11B -157.6(3)
C2B C1B C11B N11B -162.8(3)
C6B C1B C11B N11B 20.1(4)
N11B C11B O11B Cd1 15.5(3)
C1B C11B O11B Cd1 -167.0(2)
N12A Cd1 O11B C11B -149.64(19)
N12B Cd1 O11B C11B -13.7(2)
O11A Cd1 O11B C11B 162.0(2)
O1A Cd1 O11B C11B 75.5(2)
O11B C11B N11B N12B -5.8(4)
C1B C11B N11B N12B 176.6(2)
C11B N11B N12B Cd1 -7.1(3)
N12A Cd1 N12B N11B 150.76(16)
O11A Cd1 N12B N11B 1.2(3)
O11B Cd1 N12B N11B 10.11(16)
O1A Cd1 N12B N11B -113.34(17)
C6B C1B C2B C3B -1.3(4)
C11B C1B C2B C3B -178.6(3)
C1B C2B C3B C4B 0.5(5)
C1B C2B C3B N31B -178.9(2)
C4B C3B N31B O32B 0.1(5)
C2B C3B N31B O32B 179.5(3)
C4B C3B N31B O31B -179.2(3)
C2B C3B N31B O31B 0.3(5)
C2B C3B C4B C5B 0.2(5)
N31B C3B C4B C5B 179.6(3)
C3B C4B C5B C6B -0.1(5)
C4B C5B C6B C1B -0.8(5)
C2B C1B C6B C5B 1.4(4)
C11B C1B C6B C5B 178.6(3)
O3A N1A O1A Cd1 -158.5(2)
O2A N1A O1A Cd1 21.3(3)
N12A Cd1 O1A N1A -178.19(17)
N12B Cd1 O1A N1A 48.31(17)
O11A Cd1 O1A N1A -105.62(16)
O11B Cd1 O1A N1A -26.34(19)
