#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/98/2019896.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_2019896
loop_
_publ_author_name
'Shi, Wei'
'Liu, Jian-Jun'
'Ou, Xiang-Ping'
'Huang, Chang-Cang'
_publ_section_title
;
 A three-dimensional cadmium(II) coordination polymer with unequal
 homochiral double-stranded concentric helical chains
;
_journal_coeditor_code           QS3042
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615004258
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
'[Cd2 (C7 H5 N6 O)2 (C2 H3 O2) (O H)], 0.75H2 O'
_chemical_formula_moiety         'C16 H14 Cd2 N12 O5, O.75(H2 O1)'
_chemical_formula_sum            'C16 H15.5 Cd2 N12 O5.75'
_chemical_formula_weight         690.70
_chemical_name_systematic
;Poly[[(μ₂-acetato-κ³O,O':O)(hydroxido-κO)(μ₄-5-nicotinamido-1H-1,2,3,4-tetrazol-1-ido-κ⁵N¹,O:N⁴:N⁵)(μ₃-5-nicotinamido-1H-1,2,3,4-tetrazol-1-ido-κ⁴N¹,O:N²:N⁴:N⁵)dicadmium(II)]
0.75-hydrate]
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.3384(19)
_cell_length_b                   13.3384(19)
_cell_length_c                   24.957(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3845.3(11)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2002)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2002)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2002)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2004)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn 724 CCD area-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            32583
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.464
_exptl_absorpt_coefficient_mu    1.713
_exptl_absorpt_correction_T_max  0.9243
_exptl_absorpt_correction_T_min  0.8207
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(RAPID-AUTO; Rigaku, 1998)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       block
_exptl_crystal_F_000             2025
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.948
_refine_ls_abs_structure_details
;
Flack x determined using 2636 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al.,  2013)
;
_refine_ls_abs_structure_Flack   0.057(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5837
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0456
_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)+(0.0417P)²+13.0243P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                5779
_reflns_number_total             5837
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qs3042sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        3845.3(13)
_cod_database_code               2019896
_cod_database_fobs_code          2019896
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelxl_version_number           2014/6
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/6'
'-y, x-y, z+1/3'
'-x, -y, z+1/2'
'-x+y, -x, z+2/3'
'y, -x+y, z+5/6'
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
Cd Cd1 0.11549(5) 0.71693(5) 0.11990(3) 0.01890(15) Uani d 1
Cd Cd2 0.00945(5) 0.38612(5) 0.07650(3) 0.01994(15) Uani d 1
N N1 0.2764(6) 0.8412(7) 0.1656(3) 0.0236(17) Uani d 1
N N2 0.2657(7) 0.9096(7) 0.2023(3) 0.0231(16) Uani d 1
N N3 0.3654(7) 0.9740(7) 0.2245(3) 0.0224(17) Uani d 1
N N4 0.4461(6) 0.9513(7) 0.2043(3) 0.0196(15) Uani d 1
N N5 0.4320(7) 0.8202(8) 0.1319(4) 0.0289(19) Uani d 1
H H5A 0.3886 0.7764 0.1065 0.035 Uiso calc 1
N N6 0.6592(7) 0.6863(8) 0.0199(4) 0.0260(17) Uani d 1
N N7 0.1698(7) 1.4394(7) 0.0258(3) 0.0233(16) Uani d 1
N N8 0.2213(7) 1.5383(7) -0.0030(4) 0.0298(19) Uani d 1
N N9 0.2928(7) 1.5355(7) -0.0375(4) 0.0266(18) Uani d 1
N N10 0.2896(7) 1.4319(7) -0.0326(3) 0.0239(18) Uani d 1
N N11 0.1916(8) 1.2693(7) 0.0246(4) 0.032(2) Uani d 1
H H11A 0.2365 1.2456 0.0125 0.038 Uiso calc 1
N N12 0.1006(7) 0.8805(7) 0.0980(4) 0.0266(17) Uani d 1
C C1 0.3896(8) 0.8702(8) 0.1666(4) 0.0229(19) Uani d 1
C C2 0.5379(8) 0.8385(9) 0.1369(4) 0.027(2) Uani d 1
C C3 0.5770(9) 0.7818(9) 0.0956(4) 0.028(2) Uani d 1
C C4 0.5168(11) 0.7345(13) 0.0487(5) 0.048(3) Uani d 1
H H4 0.4473 0.7327 0.0421 0.058 Uiso calc 1
C C5 0.5612(10) 0.6900(13) 0.0120(5) 0.047(3) Uani d 1
H H5 0.5213 0.6609 -0.0200 0.056 Uiso calc 1
C C6 0.7129(11) 0.7292(13) 0.0652(5) 0.050(4) Uani d 1
H H6 0.7800 0.7260 0.0716 0.060 Uiso calc 1
C C7 0.6785(11) 0.7789(13) 0.1045(5) 0.046(3) Uani d 1
H H7 0.7216 0.8093 0.1356 0.055 Uiso calc 1
C C8 0.2137(9) 1.3768(8) 0.0067(4) 0.024(2) Uani d 1
C C9 0.1094(10) 1.1984(9) 0.0580(4) 0.027(2) Uani d 1
C C10 0.1086(8) 1.0878(8) 0.0713(4) 0.026(2) Uani d 1
C C11 0.0161(9) 1.0024(9) 0.1000(5) 0.035(2) Uani d 1
H H11 -0.0446 1.0128 0.1112 0.042 Uiso calc 1
C C12 0.0168(9) 0.9017(9) 0.1113(5) 0.036(3) Uani d 1
H H12 -0.0464 0.8442 0.1298 0.043 Uiso calc 1
C C13 0.1942(12) 1.0661(12) 0.0555(7) 0.063(5) Uani d 1
H H13 0.2564 1.1201 0.0352 0.076 Uiso calc 1
C C14 0.1867(13) 0.9614(12) 0.0703(7) 0.064(5) Uani d 1
H H14 0.2462 0.9485 0.0599 0.077 Uiso calc 1
C C15 0.1475(9) 0.5021(9) 0.1669(5) 0.038(3) Uani d 1
C C16 0.2206(16) 0.5707(12) 0.2148(6) 0.074(6) Uani d 1
H H16A 0.2420 0.5233 0.2353 0.111 Uiso calc 1
H H16B 0.2892 0.6383 0.2024 0.111 Uiso calc 1
H H16C 0.1767 0.5937 0.2370 0.111 Uiso calc 1
O O1 0.6132(7) 0.8948(8) 0.1730(4) 0.043(2) Uani d 1
O OW1 0.748(5) 0.787(5) 0.238(2) 0.087(9) Uiso d 0.25
O O2 0.0352(7) 1.2171(6) 0.0777(4) 0.0361(18) Uani d 1
O OW2 0.467(5) 0.524(5) 0.195(2) 0.087(9) Uiso d 0.25
O O3 0.2528(7) 0.7475(7) 0.0528(3) 0.0304(16) Uani d 1
H H3 0.244(11) 0.688(6) 0.037(4) 0.036 Uiso d 1
O OW3 0.424(5) 0.458(5) 0.142(2) 0.087(9) Uiso d 0.25
O O4 0.1113(6) 0.5452(6) 0.1358(3) 0.0298(15) Uani d 1
O O5 0.1242(7) 0.3964(6) 0.1613(4) 0.044(2) 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Cd1 O4 . . 100.6(3) y
N1 Cd1 N3 . 6_454 168.2(3) y
O4 Cd1 N3 . 6_454 83.5(3) y
N1 Cd1 N6 . 2 101.5(3) y
O4 Cd1 N6 . 2 86.5(3) y
N3 Cd1 N6 6_454 2 89.7(3) y
N1 Cd1 N12 . . 85.8(3) y
O4 Cd1 N12 . . 173.6(3) y
N3 Cd1 N12 6_454 . 90.2(3) y
N6 Cd1 N12 2 . 92.2(3) y
N1 Cd1 O3 . . 82.0(3) y
O4 Cd1 O3 . . 85.7(3) y
N3 Cd1 O3 6_454 . 87.3(3) y
N6 Cd1 O3 2 . 171.9(3) y
N12 Cd1 O3 . . 95.3(3) y
N7 Cd2 N10 1_545 2_655 163.2(3) y
N7 Cd2 O1 1_545 6_454 90.1(3) y
N10 Cd2 O1 2_655 6_454 90.2(3) y
N7 Cd2 N4 1_545 6_454 97.9(3) y
N10 Cd2 N4 2_655 6_454 98.3(3) y
O1 Cd2 N4 6_454 6_454 75.2(3) y
N7 Cd2 O4 1_545 . 92.2(3) y
N10 Cd2 O4 2_655 . 93.5(3) y
O1 Cd2 O4 6_454 . 158.7(3) y
N4 Cd2 O4 6_454 . 83.5(3) y
N7 Cd2 O2 1_545 1_545 75.6(3) y
N10 Cd2 O2 2_655 1_545 88.0(3) y
O1 Cd2 O2 6_454 1_545 78.8(3) y
N4 Cd2 O2 6_454 1_545 153.2(3) y
O4 Cd2 O2 . 1_545 122.3(3) y
N7 Cd2 O5 1_545 . 90.0(3) y
N10 Cd2 O5 2_655 . 81.3(3) y
O1 Cd2 O5 6_454 . 149.5(3) y
N4 Cd2 O5 6_454 . 134.9(3) y
O4 Cd2 O5 . . 51.8(2) y
O2 Cd2 O5 1_545 . 71.6(3) y
N2 N1 C1 . . 105.9(7) ?
N2 N1 Cd1 . . 117.1(5) ?
C1 N1 Cd1 . . 137.0(6) ?
N3 N2 N1 . . 108.5(7) ?
N2 N3 N4 . . 111.1(7) ?
N2 N3 Cd1 . 2_665 122.9(6) ?
N4 N3 Cd1 . 2_665 125.8(6) ?
C1 N4 N3 . . 104.6(7) ?
C1 N4 Cd2 . 2_665 129.4(6) ?
N3 N4 Cd2 . 2_665 124.4(6) ?
C2 N5 C1 . . 120.9(9) ?
C2 N5 H5A . . 119.5 ?
C1 N5 H5A . . 119.5 ?
C6 N6 C5 . . 116.1(9) ?
C6 N6 Cd1 . 6_554 125.7(7) ?
C5 N6 Cd1 . 6_554 118.2(7) ?
C8 N7 N8 . . 104.9(8) ?
C8 N7 Cd2 . 1_565 130.2(6) ?
N8 N7 Cd2 . 1_565 122.8(6) ?
N9 N8 N7 . . 110.3(7) ?
N8 N9 N10 . . 108.5(8) ?
C8 N10 N9 . . 104.7(7) ?
C8 N10 Cd2 . 6_564 132.8(6) ?
N9 N10 Cd2 . 6_564 122.2(6) ?
C9 N11 C8 . . 127.8(9) ?
C9 N11 H11A . . 116.1 ?
C8 N11 H11A . . 116.1 ?
C14 N12 C12 . . 116.2(9) ?
C14 N12 Cd1 . . 116.1(7) ?
C12 N12 Cd1 . . 127.7(7) ?
N4 C1 N1 . . 109.8(8) ?
N4 C1 N5 . . 129.1(8) ?
N1 C1 N5 . . 121.2(8) ?
O1 C2 N5 . . 129.3(10) ?
O1 C2 C3 . . 114.0(8) ?
N5 C2 C3 . . 116.6(9) ?
C4 C3 C7 . . 118.3(10) ?
C4 C3 C2 . . 122.5(10) ?
C7 C3 C2 . . 119.1(9) ?
C5 C4 C3 . . 119.0(11) ?
C5 C4 H4 . . 120.5 ?
C3 C4 H4 . . 120.5 ?
N6 C5 C4 . . 123.5(11) ?
N6 C5 H5 . . 118.2 ?
C4 C5 H5 . . 118.2 ?
N6 C6 C7 . . 125.6(10) ?
N6 C6 H6 . . 117.2 ?
C7 C6 H6 . . 117.2 ?
C6 C7 C3 . . 117.4(11) ?
C6 C7 H7 . . 121.3 ?
C3 C7 H7 . . 121.3 ?
N7 C8 N10 . . 111.7(8) ?
N7 C8 N11 . . 127.2(9) ?
N10 C8 N11 . . 121.0(8) ?
O2 C9 N11 . . 124.5(9) ?
O2 C9 C10 . . 119.7(9) ?
N11 C9 C10 . . 115.8(9) ?
C13 C10 C11 . . 117.9(9) ?
C13 C10 C9 . . 123.1(9) ?
C11 C10 C9 . . 119.0(9) ?
C12 C11 C10 . . 118.0(9) ?
C12 C11 H11 . . 121.0 ?
C10 C11 H11 . . 121.0 ?
N12 C12 C11 . . 125.0(10) ?
N12 C12 H12 . . 117.5 ?
C11 C12 H12 . . 117.5 ?
C10 C13 C14 . . 118.9(11) ?
C10 C13 H13 . . 120.5 ?
C14 C13 H13 . . 120.5 ?
N12 C14 C13 . . 123.8(11) ?
N12 C14 H14 . . 118.1 ?
C13 C14 H14 . . 118.1 ?
O4 C15 O5 . . 121.2(11) ?
O4 C15 C16 . . 120.6(11) ?
O5 C15 C16 . . 118.2(12) ?
C15 C16 H16A . . 109.5 ?
C15 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
C15 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
C2 O1 Cd2 . 2_665 134.5(6) ?
C9 O2 Cd2 . 1_565 132.5(7) ?
Cd1 O3 H3 . . 117(9) ?
C15 O4 Cd1 . . 140.7(7) ?
C15 O4 Cd2 . . 99.3(7) ?
Cd1 O4 Cd2 . . 120.0(3) ?
C15 O5 Cd2 . . 87.7(7) ?
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 N1 . 2.258(7) y
Cd1 O4 . 2.299(7) y
Cd1 N3 6_454 2.307(8) y
Cd1 N6 2 2.347(8) y
Cd1 N12 . 2.352(8) y
Cd1 O3 . 2.361(7) y
Cd2 N7 1_545 2.273(8) y
Cd2 N10 2_655 2.283(8) y
Cd2 O1 6_454 2.284(8) y
Cd2 N4 6_454 2.302(7) y
Cd2 O4 . 2.378(7) y
Cd2 O2 1_545 2.445(7) y
Cd2 O5 . 2.575(9) y
N1 N2 . 1.350(10) ?
N1 C1 . 1.359(11) ?
N2 N3 . 1.294(11) ?
N3 N4 . 1.354(10) ?
N3 Cd1 2_665 2.307(8) ?
N4 C1 . 1.343(12) ?
N4 Cd2 2_665 2.302(7) ?
N5 C2 . 1.314(12) ?
N5 C1 . 1.376(12) ?
N5 H5A . 0.8600 ?
N6 C6 . 1.308(15) ?
N6 C5 . 1.348(13) ?
N6 Cd1 6_554 2.347(8) ?
N7 C8 . 1.324(11) ?
N7 N8 . 1.349(11) ?
N7 Cd2 1_565 2.273(8) ?
N8 N9 . 1.301(12) ?
N9 N10 . 1.366(10) ?
N10 C8 . 1.336(12) ?
N10 Cd2 6_564 2.283(8) ?
N11 C9 . 1.325(13) ?
N11 C8 . 1.386(11) ?
N11 H11A . 0.8600 ?
N12 C14 . 1.312(15) ?
N12 C12 . 1.326(13) ?
C2 O1 . 1.278(13) ?
C2 C3 . 1.517(13) ?
C3 C4 . 1.380(16) ?
C3 C7 . 1.391(15) ?
C4 C5 . 1.377(15) ?
C4 H4 . 0.9300 ?
C5 H5 . 0.9300 ?
C6 C7 . 1.385(15) ?
C6 H6 . 0.9300 ?
C7 H7 . 0.9300 ?
C9 O2 . 1.236(12) ?
C9 C10 . 1.507(13) ?
C10 C13 . 1.368(15) ?
C10 C11 . 1.389(13) ?
C11 C12 . 1.377(14) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
C13 C14 . 1.399(16) ?
C13 H13 . 0.9300 ?
C14 H14 . 0.9300 ?
C15 O4 . 1.201(14) ?
C15 O5 . 1.290(13) ?
C15 C16 . 1.525(18) ?
C16 H16A . 0.9600 ?
C16 H16B . 0.9600 ?
C16 H16C . 0.9600 ?
O1 Cd2 2_665 2.284(8) ?
O2 Cd2 1_565 2.445(7) ?
OW2 OW3 . 1.54(7) ?
O3 H3 . 0.841(15) ?
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
N5 H5A O3 . 0.86 2.13 2.868(11) 144.1
N11 H11A O5 6_564 0.86 2.03 2.814(11) 151.4
N11 H11A O2 6_454 0.86 2.64 3.146(13) 118.7
O3 H3 N8 1_545 0.84(7) 2.11(6) 2.955(11) 179(13)
