#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/90/4319023.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_4319023
loop_
_publ_author_name
'Xiang Xue'
'Xi-Sen Wang'
'Li-Zhong Wang'
'Ren-Gen Xiong'
'Brendan F. Abrahams'
'Xiao-Zeng You'
'Zi-Ling Xue'
'Chi-Ming Che'
_publ_contact_author_address
;
Prof. Ren-Gen Xiong
Coordination Chemistry Institue
Nanjing University, Nanjing
210093, P. R. China
;
_publ_contact_author_email       xiongrg@netra.nju.edu.cn
_publ_contact_author_fax         86-25-3317761
_publ_contact_author_name        'Prof. Ren-Gen Xiong'
_publ_contact_author_phone       86-25-3594724
_publ_section_title
;
 Hydrothermal Preparation of Novel Cd(II) Coordination Polymers Employing
 5-(4-Pyridyl)tetrazolate as a Bridging Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6544
_journal_page_last               6546
_journal_paper_doi               10.1021/ic0257118
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C6 H6 Cd0.5 N5 O'
_chemical_formula_weight         220.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.4880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4360(4)
_cell_length_b                   8.0018(4)
_cell_length_c                   10.8795(5)
_cell_measurement_temperature    296(2)
_cell_volume                     731.03(6)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '0.3 wide w/ exposures'
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6765
_diffrn_reflns_theta_full        33.45
_diffrn_reflns_theta_max         33.45
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    1.528
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.757419
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.789
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.609
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.609
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                2031
_reflns_number_total             2704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0257118-2_s1_2.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C6 H6 Cd0.50 N5 O'
_cod_database_code               4319023
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 0.0000 0.0000 0.01894(8) Uani 1 2 d S . .
O1 O -0.09652(18) 0.2578(2) 0.05640(16) 0.0259(3) Uani 1 1 d . . .
H1A H -0.0709 0.2741 0.1300 0.039 Uiso 1 1 calc R . .
C6 C -0.1009(2) -0.0515(3) -0.32075(19) 0.0178(3) Uani 1 1 d . . .
C5 C 0.0326(2) -0.1434(2) -0.36487(19) 0.0191(3) Uani 1 1 d . . .
N5 N -0.2388(2) -0.0274(2) -0.3894(2) 0.0228(4) Uani 1 1 d . . .
N4 N -0.1042(2) 0.0205(2) -0.20884(19) 0.0202(3) Uani 1 1 d . . .
N3 N -0.3287(2) 0.0625(3) -0.31810(18) 0.0240(4) Uani 1 1 d . . .
C4 C 0.1879(2) -0.1278(3) -0.3098(2) 0.0242(4) Uani 1 1 d . . .
H4A H 0.2110 -0.0545 -0.2442 0.029 Uiso 1 1 calc R . .
N2 N -0.2495(2) 0.0915(2) -0.21089(17) 0.0229(3) Uani 1 1 d . . .
C3 C 0.0083(2) -0.2502(3) -0.4657(2) 0.0245(4) Uani 1 1 d . . .
H3B H -0.0924 -0.2604 -0.5080 0.029 Uiso 1 1 calc R . .
C2 C 0.3077(3) -0.2231(3) -0.3539(2) 0.0260(4) Uani 1 1 d . . .
H2B H 0.4111 -0.2103 -0.3171 0.031 Uiso 1 1 calc R . .
C1 C 0.1343(2) -0.3406(3) -0.5025(2) 0.0258(4) Uani 1 1 d . . .
H1B H 0.1154 -0.4114 -0.5701 0.031 Uiso 1 1 calc R . .
N1 N 0.2820(2) -0.3325(2) -0.44663(17) 0.0226(3) Uani 1 1 d . . .
H1 H -0.151(4) 0.323(4) 0.008(4) 0.059(10) Uiso 1 1 d . . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cd1 O1 180.00(11) 3 . ?
O1 Cd1 N4 94.86(6) 3 3 ?
O1 Cd1 N4 85.14(6) . 3 ?
O1 Cd1 N4 85.14(6) 3 . ?
O1 Cd1 N4 94.86(6) . . ?
N4 Cd1 N4 180.00(13) 3 . ?
O1 Cd1 N1 82.16(6) 3 4_556 ?
O1 Cd1 N1 97.84(6) . 4_556 ?
N4 Cd1 N1 87.22(6) 3 4_556 ?
N4 Cd1 N1 92.78(6) . 4_556 ?
O1 Cd1 N1 97.84(6) 3 2_554 ?
O1 Cd1 N1 82.16(6) . 2_554 ?
N4 Cd1 N1 92.78(6) 3 2_554 ?
N4 Cd1 N1 87.22(6) . 2_554 ?
N1 Cd1 N1 180.00(12) 4_556 2_554 ?
Cd1 O1 H1A 109.5 . . ?
Cd1 O1 H1 125(2) . . ?
H1A O1 H1 125.7 . . ?
N5 C6 N4 110.57(19) . . ?
N5 C6 C5 123.07(19) . . ?
N4 C6 C5 126.36(18) . . ?
C3 C5 C4 117.17(18) . . ?
C3 C5 C6 120.45(18) . . ?
C4 C5 C6 122.38(18) . . ?
C6 N5 N3 105.31(18) . . ?
N2 N4 C6 105.17(17) . . ?
N2 N4 Cd1 107.40(14) . . ?
C6 N4 Cd1 143.15(14) . . ?
N2 N3 N5 109.93(17) . . ?
C2 C4 C5 119.22(19) . . ?
C2 C4 H4A 120.4 . . ?
C5 C4 H4A 120.4 . . ?
N3 N2 N4 109.02(17) . . ?
C1 C3 C5 119.48(19) . . ?
C1 C3 H3B 120.3 . . ?
C5 C3 H3B 120.3 . . ?
N1 C2 C4 123.34(19) . . ?
N1 C2 H2B 118.3 . . ?
C4 C2 H2B 118.3 . . ?
N1 C1 C3 123.8(2) . . ?
N1 C1 H1B 118.1 . . ?
C3 C1 H1B 118.1 . . ?
C1 N1 C2 116.85(18) . . ?
C1 N1 Cd1 124.66(14) . 2_544 ?
C2 N1 Cd1 118.49(14) . 2_544 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O1 2.3219(16) 3 ?
Cd1 O1 2.3219(16) . ?
Cd1 N4 2.362(2) 3 ?
Cd1 N4 2.362(2) . ?
Cd1 N1 2.3912(17) 4_556 ?
Cd1 N1 2.3912(17) 2_554 ?
O1 H1A 0.8200 . ?
O1 H1 0.84(4) . ?
C6 N5 1.335(3) . ?
C6 N4 1.350(3) . ?
C6 C5 1.464(3) . ?
C5 C3 1.390(3) . ?
C5 C4 1.393(3) . ?
N5 N3 1.345(3) . ?
N4 N2 1.349(2) . ?
N3 N2 1.309(2) . ?
C4 C2 1.387(3) . ?
C4 H4A 0.9300 . ?
C3 C1 1.377(3) . ?
C3 H3B 0.9300 . ?
C2 N1 1.338(3) . ?
C2 H2B 0.9300 . ?
C1 N1 1.335(3) . ?
C1 H1B 0.9300 . ?
N1 Cd1 2.3912(17) 2_544 ?
