#------------------------------------------------------------------------------
#$Date: 2019-03-05 09:52:05 +0100 (mar 05 de mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/09/7010940.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_7010940
loop_
_publ_author_name
'Muthu, Sebastian'
'Yip, John H. K.'
'Vittal, Jagadese J.'
_publ_section_title
;
 Coordination polymers of d10 metals and
 N,N'-bis(3-pyridinecarboxamide)-1,2-ethane
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3577
_journal_paper_doi               10.1039/b105696b
_journal_year                    2001
_chemical_formula_sum            'C14 H19 Cd Cl2 N4 O13'
_chemical_formula_weight         634.63
_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                 112.487(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8353(19)
_cell_length_b                   7.5368(8)
_cell_length_c                   17.1661(17)
_cell_measurement_reflns_used    5645
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      2.45
_cell_volume                     2132.0(4)
_computing_cell_refinement       'Bruker AXS, SAINT'
_computing_data_collection       'Bruker AXS, SMART'
_computing_data_reduction        'Bruker AXS, SAINT'
_computing_molecular_graphics    'Bruker AXS, SHELXTL'
_computing_publication_material  'Bruker AXS, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_method       'ω 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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5977
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  0.9321
_exptl_absorpt_correction_T_min  0.6500
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.767
_refine_diff_density_min         -1.812
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         1884
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0489
_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)+(0.0600P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                1413
_reflns_number_total             1884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105696b.txt
_cod_data_source_block           1149
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7010940
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_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 0.5000 0.20885(8) 0.2500 0.0604(3) Uani 1 2 d S . .
O1 O 0.4280(2) 0.2540(5) 0.6100(2) 0.0510(11) Uani 1 1 d . . .
O2 O 0.5000 0.5084(7) 0.2500 0.0510(14) Uani 1 2 d SD . .
H2 H 0.478(9) 0.592(16) 0.205(7) 0.111 Uiso 0.50 1 d PD . .
O3 O 0.5911(2) -0.0144(6) 0.2718(3) 0.0586(11) Uani 1 1 d D . .
H3A H 0.597(3) -0.118(4) 0.305(2) 0.032 Uiso 1 1 d D . .
H3B H 0.643(3) -0.013(11) 0.268(7) 0.213 Uiso 1 1 d D . .
N1 N 0.5275(3) 0.2311(5) 0.3899(3) 0.0393(11) Uani 1 1 d . . .
N2 N 0.3421(3) 0.1761(7) 0.4819(3) 0.0521(14) Uani 1 1 d . . .
H2A H 0.331(4) 0.171(9) 0.431(4) 0.07(2) Uiso 1 1 d . . .
C1 C 0.6019(4) 0.2661(8) 0.4441(4) 0.0505(16) Uani 1 1 d . . .
H1 H 0.6441 0.2756 0.4241 0.061 Uiso 1 1 calc R . .
C2B C 0.6196(4) 0.2893(8) 0.5293(4) 0.0520(15) Uani 1 1 d . . .
H2' H 0.6729 0.3137 0.5667 0.062 Uiso 1 1 calc R . .
C3 C 0.5579(3) 0.2759(7) 0.5584(3) 0.0374(12) Uani 1 1 d . . .
H3 H 0.5687 0.2910 0.6160 0.045 Uiso 1 1 calc R . .
C4 C 0.4807(3) 0.2404(6) 0.5032(3) 0.0308(11) Uani 1 1 d . . .
C5 C 0.4677(3) 0.2191(7) 0.4180(3) 0.0378(12) Uani 1 1 d . . .
H5 H 0.4148 0.1953 0.3792 0.045 Uiso 1 1 calc R . .
C6 C 0.4140(3) 0.2240(7) 0.5352(3) 0.0340(12) Uani 1 1 d . . .
C7 C 0.2710(3) 0.1627(9) 0.5040(4) 0.0523(15) Uani 1 1 d . . .
H7A H 0.2879 0.1199 0.5621 0.063 Uiso 1 1 calc R . .
H7B H 0.2331 0.0760 0.4669 0.063 Uiso 1 1 calc R . .
Cl1 Cl 0.70928(7) 0.47008(17) 0.26897(7) 0.0377(3) Uani 1 1 d D . .
O4 O 0.6733(3) 0.6301(6) 0.2821(3) 0.0703(13) Uani 1 1 d D . .
O5 O 0.6946(2) 0.4501(6) 0.1826(2) 0.0551(11) Uani 1 1 d D . .
O6 O 0.6752(3) 0.3206(6) 0.2955(3) 0.0683(13) Uani 1 1 d D . .
O7 O 0.7953(2) 0.4760(7) 0.3156(2) 0.0669(13) Uani 1 1 d 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'
Cl Cl 0.1484 0.1585 '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
O2 Cd1 N1 85.75(11) . . ?
O2 Cd1 N1 85.75(10) . 2_655 ?
N1 Cd1 N1 171.5(2) . 2_655 ?
O2 Cd1 O3 137.86(11) . 2_655 ?
N1 Cd1 O3 94.64(15) . 2_655 ?
N1 Cd1 O3 91.66(15) 2_655 2_655 ?
O2 Cd1 O3 137.86(11) . . ?
N1 Cd1 O3 91.66(15) . . ?
N1 Cd1 O3 94.64(15) 2_655 . ?
O3 Cd1 O3 84.3(2) 2_655 . ?
C1 N1 C5 119.1(4) . . ?
C1 N1 Cd1 120.8(3) . . ?
C5 N1 Cd1 120.0(4) . . ?
C6 N2 C7 123.6(5) . . ?
N1 C1 C2B 121.9(5) . . ?
C3 C2B C1 119.0(6) . . ?
C4 C3 C2B 119.8(5) . . ?
C3 C4 C5 117.9(4) . . ?
C3 C4 C6 119.6(4) . . ?
C5 C4 C6 122.5(5) . . ?
N1 C5 C4 122.3(5) . . ?
O1 C6 N2 122.2(5) . . ?
O1 C6 C4 119.7(5) . . ?
N2 C6 C4 118.0(4) . . ?
N2 C7 C7 111.8(7) . 7_556 ?
O5 Cl1 O4 110.0(3) . . ?
O5 Cl1 O7 108.6(2) . . ?
O4 Cl1 O7 109.6(3) . . ?
O5 Cl1 O6 108.6(3) . . ?
O4 Cl1 O6 110.1(3) . . ?
O7 Cl1 O6 109.9(3) . . ?
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 O2 2.257(5) . ?
Cd1 N1 2.266(4) . ?
Cd1 N1 2.266(4) 2_655 ?
Cd1 O3 2.269(4) 2_655 ?
Cd1 O3 2.269(4) . ?
O1 C6 1.232(6) . ?
N1 C1 1.324(8) . ?
N1 C5 1.332(7) . ?
N2 C6 1.310(7) . ?
N2 C7 1.459(7) . ?
C1 C2B 1.385(8) . ?
C2B C3 1.374(8) . ?
C3 C4 1.366(7) . ?
C4 C5 1.399(6) . ?
C4 C6 1.495(7) . ?
C7 C7 1.495(12) 7_556 ?
Cl1 O5 1.412(4) . ?
Cl1 O4 1.424(4) . ?
Cl1 O7 1.434(4) . ?
Cl1 O6 1.435(4) . ?
