#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/71/2227158.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_2227158
loop_
_publ_author_name
'Chen, Man-Sheng'
'Deng, Yi-Fang'
'Zhang, Chun-Hua'
'Kuang, Dai-Zhi'
_publ_section_title
;
 catena-Poly[[[diaquacadmium(II)]-bis[μ-3,5-bis(isonicotinamido)benzoato]]
 tetrahydrate]
;
_journal_coeditor_code           BG2362
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1253
_journal_page_last               m1254
_journal_paper_doi               10.1107/S1600536810036147
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cd (C19 H13 N4 O4)2 (H2 O)2], 4H2 O'
_chemical_formula_moiety         'C38 H30 Cd N8 O10, 4(H2 O)'
_chemical_formula_sum            'C38 H38 Cd N8 O14'
_chemical_formula_weight         943.16
_chemical_name_systematic
;
catena-Poly[[[diaquacadmium(II)]-bis[μ-3,5-
bis(isonicotinamido)benzoato]] tetrahydrate]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.801(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.584(3)
_cell_length_b                   10.8568(19)
_cell_length_c                   21.891(4)
_cell_measurement_reflns_used    3272
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.31
_cell_volume                     4058.5(12)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10338
_diffrn_reflns_theta_full        25.75
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.9409
_exptl_absorpt_correction_T_min  0.8867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.480
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         3867
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0527P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1101
_reflns_number_gt                3391
_reflns_number_total             3867
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bg2362.cif
_cod_data_source_block           I
_cod_database_code               2227158
_cod_database_fobs_code          2227158
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd Cd1 0.0000 0.74023(3) -0.2500 0.03203(14) Uani d SU 1 . .
C C1 0.1391(2) 0.6471(3) -0.14433(15) 0.0341(8) Uani d . 1 . .
C C2 0.16577(18) 0.6286(3) -0.07425(14) 0.0304(7) Uani d . 1 . .
C C3 0.21138(19) 0.5274(3) -0.04962(15) 0.0340(8) Uani d . 1 . .
H H3A 0.2266 0.4705 -0.0762 0.041 Uiso calc R 1 . .
C C4 0.23363(19) 0.5125(3) 0.01481(16) 0.0334(8) Uani d . 1 . .
C C5 0.2124(2) 0.5954(3) 0.05570(15) 0.0360(8) Uani d . 1 . .
H H5 0.2276 0.5832 0.0990 0.043 Uiso calc R 1 . .
C C6 0.16780(19) 0.6977(3) 0.03069(15) 0.0312(7) Uani d . 1 . .
C C7 0.14483(19) 0.7127(3) -0.03395(15) 0.0316(7) Uani d . 1 . .
H H7 0.1147 0.7807 -0.0505 0.038 Uiso calc R 1 . .
C C8 0.3530(2) 0.3931(3) 0.03346(16) 0.0390(8) Uani d . 1 . .
C C9 0.3967(2) 0.2847(3) 0.06802(18) 0.0406(9) Uani d . 1 . .
C C10 0.4431(2) 0.2140(4) 0.0395(2) 0.0550(11) Uani d . 1 . .
H H10 0.4453 0.2292 -0.0018 0.066 Uiso calc R 1 . .
C C11 0.4868(3) 0.1191(4) 0.0739(2) 0.0638(13) Uani d . 1 . .
H H11 0.5172 0.0701 0.0541 0.077 Uiso calc R 1 . .
C C12 0.4417(3) 0.1640(4) 0.1594(2) 0.0609(12) Uani d . 1 . .
H H12 0.4406 0.1472 0.2008 0.073 Uiso calc R 1 . .
C C13 0.3957(3) 0.2595(3) 0.1292(2) 0.0532(11) Uani d . 1 . .
H H13 0.3648 0.3054 0.1499 0.064 Uiso calc R 1 . .
C C14 0.1521(2) 0.7883(3) 0.13085(16) 0.0372(8) Uani d . 1 . .
C C15 0.1209(2) 0.9006(3) 0.15632(15) 0.0352(8) Uani d . 1 . .
C C16 0.1481(3) 0.9300(4) 0.21868(17) 0.0524(11) Uani d . 1 . .
H H16 0.1864 0.8819 0.2446 0.063 Uiso calc R 1 . .
C C17 0.1180(3) 1.0315(4) 0.24232(18) 0.0534(11) Uani d . 1 . .
H H17 0.1380 1.0517 0.2844 0.064 Uiso calc R 1 . .
C C18 0.0367(2) 1.0727(4) 0.14846(17) 0.0487(10) Uani d . 1 . .
H H18 -0.0018 1.1220 0.1236 0.058 Uiso calc R 1 . .
C C19 0.0636(2) 0.9741(3) 0.12058(17) 0.0460(9) Uani d . 1 . .
H H19 0.0433 0.9572 0.0782 0.055 Uiso calc R 1 . .
N N1 0.4871(2) 0.0953(3) 0.13331(19) 0.0625(10) Uani d . 1 . .
N N2 0.06210(18) 1.1019(3) 0.20837(13) 0.0398(7) Uani d . 1 . .
N N3 0.28104(17) 0.4100(3) 0.04134(13) 0.0402(7) Uani d . 1 . .
H H3 0.2624 0.3573 0.0632 0.048 Uiso calc R 1 . .
N N4 0.14702(16) 0.7905(3) 0.06830(12) 0.0353(7) Uani d . 1 . .
H H4 0.1288 0.8572 0.0491 0.042 Uiso calc R 1 . .
O O1 0.09323(16) 0.7351(2) -0.16214(11) 0.0429(6) Uani d . 1 . .
O O2 0.16316(16) 0.5753(2) -0.17948(11) 0.0505(7) Uani d . 1 . .
O O3 0.38414(17) 0.4597(2) 0.00154(13) 0.0585(8) Uani d . 1 . .
O O4 0.17829(19) 0.7016(2) 0.16454(12) 0.0571(8) Uani d . 1 . .
O O5 0.07154(19) 0.6011(3) -0.29733(14) 0.0501(7) Uani d DU 1 . .
O O6 0.1941(3) 0.3124(5) 0.1269(2) 0.1053(14) Uani d DU 1 . .
O O7 0.2760(3) 0.1472(3) 0.20727(17) 0.0782(11) Uani d D 1 . .
H H5A 0.050(2) 0.539(3) -0.3152(17) 0.055(13) Uiso d D 1 . .
H H7B 0.299(3) 0.154(6) 0.2454(12) 0.12(2) Uiso d D 1 . .
H H7A 0.283(3) 0.073(2) 0.198(2) 0.11(2) Uiso d D 1 . .
H H5B 0.109(2) 0.575(4) -0.2698(18) 0.088(19) Uiso d D 1 . .
H H6B 0.150(2) 0.325(7) 0.135(3) 0.16(3) Uiso d D 1 . .
H H6A 0.207(4) 0.243(3) 0.143(3) 0.112(6) Uiso d DU 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'
Cd Cd -0.8075 1.2024 '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'
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
O1 Cd1 O1 . 2_554 177.13(12) ?
O1 Cd1 N2 . 5_575 89.86(9) ?
O1 Cd1 N2 2_554 5_575 92.25(10) ?
O1 Cd1 N2 . 6_575 92.25(10) ?
O1 Cd1 N2 2_554 6_575 89.86(9) ?
N2 Cd1 N2 5_575 6_575 85.36(15) ?
O1 Cd1 O5 . 2_554 87.95(10) ?
O1 Cd1 O5 2_554 2_554 90.21(10) ?
N2 Cd1 O5 5_575 2_554 87.17(11) ?
N2 Cd1 O5 6_575 2_554 172.53(10) ?
O1 Cd1 O5 . . 90.21(10) ?
O1 Cd1 O5 2_554 . 87.95(10) ?
N2 Cd1 O5 5_575 . 172.53(10) ?
N2 Cd1 O5 6_575 . 87.17(11) ?
O5 Cd1 O5 2_554 . 100.30(15) ?
O2 C1 O1 . . 125.3(3) ?
O2 C1 C2 . . 118.7(3) ?
O1 C1 C2 . . 116.1(3) ?
C7 C2 C3 . . 119.5(3) ?
C7 C2 C1 . . 119.8(3) ?
C3 C2 C1 . . 120.7(3) ?
C4 C3 C2 . . 119.0(3) ?
C4 C3 H3A . . 120.5 ?
C2 C3 H3A . . 120.5 ?
C3 C4 C5 . . 122.1(3) ?
C3 C4 N3 . . 120.2(3) ?
C5 C4 N3 . . 117.7(3) ?
C4 C5 C6 . . 118.5(3) ?
C4 C5 H5 . . 120.7 ?
C6 C5 H5 . . 120.7 ?
C7 C6 C5 . . 119.6(3) ?
C7 C6 N4 . . 117.5(3) ?
C5 C6 N4 . . 122.9(3) ?
C2 C7 C6 . . 121.2(3) ?
C2 C7 H7 . . 119.4 ?
C6 C7 H7 . . 119.4 ?
O3 C8 N3 . . 124.2(3) ?
O3 C8 C9 . . 120.3(3) ?
N3 C8 C9 . . 115.5(3) ?
C13 C9 C10 . . 118.7(3) ?
C13 C9 C8 . . 121.5(3) ?
C10 C9 C8 . . 119.7(4) ?
C9 C10 C11 . . 118.6(4) ?
C9 C10 H10 . . 120.7 ?
C11 C10 H10 . . 120.7 ?
N1 C11 C10 . . 123.1(4) ?
N1 C11 H11 . . 118.5 ?
C10 C11 H11 . . 118.5 ?
N1 C12 C13 . . 124.4(4) ?
N1 C12 H12 . . 117.8 ?
C13 C12 H12 . . 117.8 ?
C9 C13 C12 . . 118.2(4) ?
C9 C13 H13 . . 120.9 ?
C12 C13 H13 . . 120.9 ?
O4 C14 N4 . . 123.5(3) ?
O4 C14 C15 . . 121.6(3) ?
N4 C14 C15 . . 114.9(3) ?
C16 C15 C19 . . 117.8(3) ?
C16 C15 C14 . . 119.2(3) ?
C19 C15 C14 . . 123.0(3) ?
C15 C16 C17 . . 119.1(4) ?
C15 C16 H16 . . 120.5 ?
C17 C16 H16 . . 120.5 ?
N2 C17 C16 . . 123.5(4) ?
N2 C17 H17 . . 118.2 ?
C16 C17 H17 . . 118.2 ?
N2 C18 C19 . . 124.0(3) ?
N2 C18 H18 . . 118.0 ?
C19 C18 H18 . . 118.0 ?
C15 C19 C18 . . 118.9(3) ?
C15 C19 H19 . . 120.5 ?
C18 C19 H19 . . 120.5 ?
C12 N1 C11 . . 117.0(4) ?
C18 N2 C17 . . 116.7(3) ?
C18 N2 Cd1 . 5_575 119.1(2) ?
C17 N2 Cd1 . 5_575 124.0(2) ?
C8 N3 C4 . . 122.4(3) ?
C8 N3 H3 . . 118.8 ?
C4 N3 H3 . . 118.8 ?
C14 N4 C6 . . 128.2(3) ?
C14 N4 H4 . . 115.9 ?
C6 N4 H4 . . 115.9 ?
C1 O1 Cd1 . . 125.4(2) ?
Cd1 O5 H5A . . 120(3) ?
Cd1 O5 H5B . . 109(3) ?
H5A O5 H5B . . 105(4) ?
H6B O6 H6A . . 104(6) ?
H7B O7 H7A . . 104(5) ?
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 O1 . 2.210(2) ?
Cd1 O1 2_554 2.210(2) ?
Cd1 N2 5_575 2.331(3) ?
Cd1 N2 6_575 2.331(3) ?
Cd1 O5 2_554 2.358(3) ?
Cd1 O5 . 2.358(3) ?
C1 O2 . 1.239(4) ?
C1 O1 . 1.252(4) ?
C1 C2 . 1.507(4) ?
C2 C7 . 1.379(4) ?
C2 C3 . 1.391(4) ?
C3 C4 . 1.380(4) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.382(4) ?
C4 N3 . 1.428(4) ?
C5 C6 . 1.394(4) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.386(4) ?
C6 N4 . 1.404(4) ?
C7 H7 . 0.9300 ?
C8 O3 . 1.222(4) ?
C8 N3 . 1.330(4) ?
C8 C9 . 1.507(5) ?
C9 C13 . 1.372(6) ?
C9 C10 . 1.373(6) ?
C10 C11 . 1.394(5) ?
C10 H10 . 0.9300 ?
C11 N1 . 1.325(5) ?
C11 H11 . 0.9300 ?
C12 N1 . 1.318(5) ?
C12 C13 . 1.382(5) ?
C12 H12 . 0.9300 ?
C13 H13 . 0.9300 ?
C14 O4 . 1.217(4) ?
C14 N4 . 1.351(4) ?
C14 C15 . 1.498(5) ?
C15 C16 . 1.372(5) ?
C15 C19 . 1.374(5) ?
C16 C17 . 1.376(5) ?
C16 H16 . 0.9300 ?
C17 N2 . 1.325(5) ?
C17 H17 . 0.9300 ?
C18 N2 . 1.319(4) ?
C18 C19 . 1.371(5) ?
C18 H18 . 0.9300 ?
C19 H19 . 0.9300 ?
N2 Cd1 5_575 2.331(3) ?
N3 H3 . 0.8600 ?
N4 H4 . 0.8600 ?
O5 H5A . 0.829(19) ?
O5 H5B . 0.83(3) ?
O6 H6B . 0.84(2) ?
O6 H6A . 0.83(2) ?
O7 H7B . 0.84(2) ?
O7 H7A . 0.85(2) ?
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
N3 H3 O6 . 0.86 2.10 2.885(5) 151.4
N4 H4 O3 7_565 0.86 2.26 3.096(4) 164.2
O5 H5B O2 . 0.83(3) 1.98(3) 2.710(4) 145(4)
O5 H5A N1 8_455 0.83(2) 2.00(2) 2.825(4) 172(4)
O6 H6B O5 6_566 0.84(2) 2.40(4) 3.163(6) 151(6)
O6 H6A O7 . 0.82(3) 1.92(4) 2.681(6) 148(5)
O7 H7A O2 7 0.85(2) 1.96(3) 2.767(4) 162(5)
O7 H7B O4 4_545 0.84(2) 1.99(3) 2.791(4) 159(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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O2 C1 C2 C7 . . . . 175.0(3) ?
O1 C1 C2 C7 . . . . -5.5(5) ?
O2 C1 C2 C3 . . . . -5.1(5) ?
O1 C1 C2 C3 . . . . 174.5(3) ?
C7 C2 C3 C4 . . . . 1.0(5) ?
C1 C2 C3 C4 . . . . -179.0(3) ?
C2 C3 C4 C5 . . . . -0.4(5) ?
C2 C3 C4 N3 . . . . -179.4(3) ?
C3 C4 C5 C6 . . . . -0.7(5) ?
N3 C4 C5 C6 . . . . 178.4(3) ?
C4 C5 C6 C7 . . . . 1.1(5) ?
C4 C5 C6 N4 . . . . -176.4(3) ?
C3 C2 C7 C6 . . . . -0.6(5) ?
C1 C2 C7 C6 . . . . 179.4(3) ?
C5 C6 C7 C2 . . . . -0.5(5) ?
N4 C6 C7 C2 . . . . 177.1(3) ?
O3 C8 C9 C13 . . . . 135.5(4) ?
N3 C8 C9 C13 . . . . -43.5(5) ?
O3 C8 C9 C10 . . . . -40.0(5) ?
N3 C8 C9 C10 . . . . 141.0(4) ?
C13 C9 C10 C11 . . . . 0.4(6) ?
C8 C9 C10 C11 . . . . 176.0(4) ?
C9 C10 C11 N1 . . . . -1.5(7) ?
C10 C9 C13 C12 . . . . 0.2(6) ?
C8 C9 C13 C12 . . . . -175.3(4) ?
N1 C12 C13 C9 . . . . 0.2(7) ?
O4 C14 C15 C16 . . . . 25.7(6) ?
N4 C14 C15 C16 . . . . -155.7(3) ?
O4 C14 C15 C19 . . . . -151.8(4) ?
N4 C14 C15 C19 . . . . 26.8(5) ?
C19 C15 C16 C17 . . . . -0.9(6) ?
C14 C15 C16 C17 . . . . -178.5(4) ?
C15 C16 C17 N2 . . . . 1.8(7) ?
C16 C15 C19 C18 . . . . 0.3(6) ?
C14 C15 C19 C18 . . . . 177.8(4) ?
N2 C18 C19 C15 . . . . -0.5(6) ?
C13 C12 N1 C11 . . . . -1.2(7) ?
C10 C11 N1 C12 . . . . 1.9(7) ?
C19 C18 N2 C17 . . . . 1.3(6) ?
C19 C18 N2 Cd1 . . . 5_575 -173.3(3) ?
C16 C17 N2 C18 . . . . -1.9(6) ?
C16 C17 N2 Cd1 . . . 5_575 172.4(3) ?
O3 C8 N3 C4 . . . . -2.7(6) ?
C9 C8 N3 C4 . . . . 176.3(3) ?
C3 C4 N3 C8 . . . . 62.3(5) ?
C5 C4 N3 C8 . . . . -116.8(4) ?
O4 C14 N4 C6 . . . . 1.7(6) ?
C15 C14 N4 C6 . . . . -176.9(3) ?
C7 C6 N4 C14 . . . . 169.1(3) ?
C5 C6 N4 C14 . . . . -13.4(6) ?
O2 C1 O1 Cd1 . . . . 31.5(5) ?
C2 C1 O1 Cd1 . . . . -148.0(2) ?
N2 Cd1 O1 C1 5_575 . . . 160.5(3) ?
N2 Cd1 O1 C1 6_575 . . . -114.2(3) ?
O5 Cd1 O1 C1 2_554 . . . 73.3(3) ?
O5 Cd1 O1 C1 . . . . -27.0(3) ?
