#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/30/1513030.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_1513030
loop_
_publ_author_name
'Jens Hunger'
_publ_section_title
;
 Synthesis and structure of coordination polymers of Mn2+, Cu2+, Ag+, Zn2+
 and Cd2+ by combination of bipyrazole and diphenate ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              60
_journal_page_last               68
_journal_paper_doi               10.1016/j.ica.2012.11.019
_journal_volume                  397
_journal_year                    2013
_chemical_formula_moiety         'C24 H22 Cd N4 O4'
_chemical_formula_sum            'C24 H22 Cd N4 O4'
_chemical_formula_weight         542.86
_chemical_name_systematic
;
catena-((μ₂-Biphenyl-2,2'-dicarboxylato)-(μ₂-3,3',5,5'-tetramethyl-
4,4'-bipyrazole)-cadmium(ii))
;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   12.1793(6)
_cell_length_b                   12.1793(6)
_cell_length_c                   26.9353(13)
_cell_measurement_reflns_used    7931
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26.9
_cell_measurement_theta_min      7.1
_cell_volume                     3460.2(3)
_computing_cell_refinement       'RECIPE (Stoe & Cie, 2002)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 2002)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 and DIAMOND'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Stoe IPDS-I'
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20191
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.86
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.8131
_exptl_absorpt_correction_T_min  0.7493
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[X-RED32 (Stoe & Cie, 2001);
crystal description using FACEIT (Stoe & Cie, 2002);
optimization using equivalent reflections
(X-SHAPE; Stoe & Cie, 1999)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.041(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.808
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4873
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.809
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0201
_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)+(0.0462P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0436
_reflns_number_gt                3942
_reflns_number_total             4873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-397-60-68-5.cif
_cod_data_source_block           5
_cod_database_code               1513030
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'
'y, x, -z'
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
C1 C 0.6943(2) -0.1085(2) 0.22319(11) 0.0221(6) Uani 1 1 d .
C2 C 0.7144(2) -0.0053(2) 0.19387(11) 0.0200(6) Uani 1 1 d .
C3 C 0.7077(3) 0.0807(2) 0.22781(11) 0.0233(6) Uani 1 1 d .
C4 C 0.6934(3) -0.2292(3) 0.21145(12) 0.0364(8) Uani 1 1 d .
H4A H 0.7592 -0.2324 0.2299 0.055 Uiso 1 1 calc R
H4B H 0.7078 -0.2323 0.1766 0.055 Uiso 1 1 calc R
H4C H 0.6127 -0.3003 0.2203 0.055 Uiso 1 1 calc R
C5 C 0.7223(3) 0.2079(3) 0.21582(12) 0.0350(7) Uani 1 1 d .
H5A H 0.6517 0.2126 0.2292 0.053 Uiso 1 1 calc R
H5B H 0.7250 0.2187 0.1805 0.053 Uiso 1 1 calc R
H5C H 0.7995 0.2735 0.2302 0.053 Uiso 1 1 calc R
C6 C 0.8503(3) 0.4874(3) 0.31041(14) 0.0355(8) Uani 1 1 d .
C7 C 0.9302(3) 0.4499(3) 0.33197(12) 0.0308(7) Uani 1 1 d .
C8 C 0.8490(3) 0.3250(3) 0.35004(12) 0.0291(7) Uani 1 1 d .
C9 C 0.8783(3) 0.6066(4) 0.28392(17) 0.0619(12) Uani 1 1 d .
H9A H 0.8206 0.5864 0.2566 0.093 Uiso 1 1 calc R
H9B H 0.9637 0.6478 0.2716 0.093 Uiso 1 1 calc R
H9C H 0.8686 0.6622 0.3065 0.093 Uiso 1 1 calc R
C10 C 0.8837(3) 0.2405(3) 0.37750(12) 0.0381(7) Uani 1 1 d .
H10A H 0.8213 0.1951 0.4027 0.057 Uiso 1 1 calc R
H10B H 0.9652 0.2907 0.3927 0.057 Uiso 1 1 calc R
H10C H 0.8868 0.1814 0.3548 0.057 Uiso 1 1 calc R
C11 C 0.5272(2) -0.0619(3) 0.41397(11) 0.0245(6) Uani 1 1 d .
C12 C 0.5039(3) -0.1421(3) 0.45984(12) 0.0259(7) Uani 1 1 d .
C13 C 0.3928(3) -0.1840(3) 0.48729(13) 0.0348(8) Uani 1 1 d .
H13 H 0.3320 -0.1646 0.4764 0.042 Uiso 1 1 calc R
C14 C 0.3712(3) -0.2539(3) 0.53040(13) 0.0413(9) Uani 1 1 d .
H14 H 0.2962 -0.2820 0.5481 0.050 Uiso 1 1 calc R
C15 C 0.4622(3) -0.2814(4) 0.54689(14) 0.0462(9) Uani 1 1 d .
H15 H 0.4491 -0.3273 0.5760 0.055 Uiso 1 1 calc R
C16 C 0.5730(3) -0.2405(3) 0.52007(13) 0.0421(8) Uani 1 1 d .
H16 H 0.6334 -0.2599 0.5314 0.051 Uiso 1 1 calc R
C17 C 0.5956(3) -0.1712(3) 0.47659(9) 0.0282(5) Uani 1 1 d .
C18 C 0.2797(3) 0.1590(3) 0.21711(11) 0.0277(7) Uani 1 1 d .
C19 C 0.1725(3) 0.1543(3) 0.19620(13) 0.0350(8) Uani 1 1 d .
H19 H 0.1798 0.1949 0.1661 0.042 Uiso 1 1 calc R
C20 C 0.0548(3) 0.0901(3) 0.21958(13) 0.0394(8) Uani 1 1 d .
H20 H -0.0154 0.0883 0.2050 0.047 Uiso 1 1 calc R
C21 C 0.0420(3) 0.0297(3) 0.26397(12) 0.0382(8) Uani 1 1 d .
H21 H -0.0366 -0.0134 0.2795 0.046 Uiso 1 1 calc R
C22 C 0.1476(3) 0.0334(3) 0.28563(13) 0.0334(7) Uani 1 1 d .
H22 H 0.1391 -0.0068 0.3159 0.040 Uiso 1 1 calc R
C23 C 0.2659(2) 0.0967(2) 0.26258(12) 0.0257(7) Uani 1 1 d .
C24 C 0.3739(3) 0.0902(3) 0.28732(12) 0.0266(7) Uani 1 1 d .
N1 N 0.6849(2) 0.03427(19) 0.27390(9) 0.0279(5) Uani 1 1 d .
N2 N 0.6770(2) -0.0817(2) 0.27034(11) 0.0269(6) Uani 1 1 d D
N3 N 0.7279(2) 0.2898(2) 0.34013(9) 0.0291(6) Uani 1 1 d .
N4 N 0.7316(3) 0.3905(2) 0.31595(10) 0.0333(6) Uani 1 1 d D
O1 O 0.4850(3) -0.11375(18) 0.37287(8) 0.0530(7) Uani 1 1 d .
O2 O 0.5881(2) 0.0548(2) 0.41753(9) 0.0531(7) Uani 1 1 d .
O3 O 0.4481(2) 0.0717(2) 0.26197(9) 0.0440(6) Uani 1 1 d .
O4 O 0.3838(2) 0.1002(2) 0.33397(9) 0.0435(6) Uani 1 1 d .
Cd1 Cd 0.572089(19) 0.08283(2) 0.330951(8) 0.02610(5) Uani 1 1 d .
H2N H 0.661(2) -0.133(3) 0.2912(11) 0.022(8) Uiso 1 1 d D
H4N H 0.671(3) 0.395(3) 0.3112(13) 0.044(11) Uiso 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'
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_3
N2 C1 C2 107.0(2) .
N2 C1 C4 120.6(2) .
C2 C1 C4 132.4(3) .
C1 C2 C3 104.5(2) .
C1 C2 C2 128.5(3) 4
C3 C2 C2 126.3(3) 4
N1 C3 C2 111.2(2) .
N1 C3 C5 121.9(3) .
C2 C3 C5 126.8(3) .
C1 C4 H4A 109.5 .
C1 C4 H4B 109.5 .
H4A C4 H4B 109.5 .
C1 C4 H4C 109.5 .
H4A C4 H4C 109.5 .
H4B C4 H4C 109.5 .
C3 C5 H5A 109.5 .
C3 C5 H5B 109.5 .
H5A C5 H5B 109.5 .
C3 C5 H5C 109.5 .
H5A C5 H5C 109.5 .
H5B C5 H5C 109.5 .
N4 C6 C7 106.7(3) .
N4 C6 C9 122.0(3) .
C7 C6 C9 131.3(3) .
C6 C7 C8 105.5(2) .
C6 C7 C7 128.7(2) 5_765
C8 C7 C7 125.7(2) 5_765
N3 C8 C7 109.8(2) .
N3 C8 C10 121.6(3) .
C7 C8 C10 128.5(3) .
C6 C9 H9A 109.5 .
C6 C9 H9B 109.5 .
H9A C9 H9B 109.5 .
C6 C9 H9C 109.5 .
H9A C9 H9C 109.5 .
H9B C9 H9C 109.5 .
C8 C10 H10A 109.5 .
C8 C10 H10B 109.5 .
H10A C10 H10B 109.5 .
C8 C10 H10C 109.5 .
H10A C10 H10C 109.5 .
H10B C10 H10C 109.5 .
O2 C11 O1 120.6(3) .
O2 C11 C12 119.4(3) .
O1 C11 C12 120.0(3) .
O2 C11 Cd1 60.61(15) .
O1 C11 Cd1 59.99(15) .
C12 C11 Cd1 179.22(18) .
C13 C12 C17 119.1(3) .
C13 C12 C11 120.2(2) .
C17 C12 C11 120.7(2) .
C14 C13 C12 121.4(3) .
C14 C13 H13 119.3 .
C12 C13 H13 119.3 .
C15 C14 C13 119.3(3) .
C15 C14 H14 120.4 .
C13 C14 H14 120.4 .
C14 C15 C16 120.1(3) .
C14 C15 H15 120.0 .
C16 C15 H15 120.0 .
C15 C16 C17 121.3(3) .
C15 C16 H16 119.3 .
C17 C16 H16 119.3 .
C16 C17 C12 118.9(3) .
C16 C17 C18 120.5(3) 5_655
C12 C17 C18 120.5(2) 5_655
C19 C18 C23 118.2(3) .
C19 C18 C17 118.0(3) 5_665
C23 C18 C17 123.8(2) 5_665
C20 C19 C18 121.2(3) .
C20 C19 H19 119.4 .
C18 C19 H19 119.4 .
C21 C20 C19 120.3(3) .
C21 C20 H20 119.9 .
C19 C20 H20 119.9 .
C20 C21 C22 119.6(3) .
C20 C21 H21 120.2 .
C22 C21 H21 120.2 .
C21 C22 C23 120.9(3) .
C21 C22 H22 119.5 .
C23 C22 H22 119.5 .
C22 C23 C18 119.8(3) .
C22 C23 C24 117.4(3) .
C18 C23 C24 122.7(3) .
O3 C24 O4 121.5(3) .
O3 C24 C23 120.0(3) .
O4 C24 C23 118.5(3) .
O3 C24 Cd1 59.57(16) .
O4 C24 Cd1 62.04(15) .
C23 C24 Cd1 178.8(2) .
C3 N1 N2 105.3(2) .
C3 N1 Cd1 122.06(19) .
N2 N1 Cd1 124.19(17) .
C1 N2 N1 112.0(2) .
C1 N2 H2N 119(2) .
N1 N2 H2N 129(2) .
C8 N3 N4 105.6(2) .
C8 N3 Cd1 123.23(18) .
N4 N3 Cd1 124.99(18) .
C6 N4 N3 112.3(3) .
C6 N4 H4N 125(2) .
N3 N4 H4N 122(3) .
C11 O1 Cd1 92.76(17) .
C11 O2 Cd1 92.51(17) .
C24 O3 Cd1 93.4(2) .
C24 O4 Cd1 90.37(16) .
N3 Cd1 N1 94.67(8) .
N3 Cd1 O3 107.67(9) .
N1 Cd1 O3 84.69(8) .
N3 Cd1 O1 140.26(8) .
N1 Cd1 O1 94.63(8) .
O3 Cd1 O1 111.61(8) .
N3 Cd1 O2 88.28(8) .
N1 Cd1 O2 120.64(9) .
O3 Cd1 O2 149.47(9) .
O1 Cd1 O2 54.12(7) .
N3 Cd1 O4 101.61(8) .
N1 Cd1 O4 138.97(8) .
O3 Cd1 O4 54.57(8) .
O1 Cd1 O4 96.22(9) .
O2 Cd1 O4 97.45(8) .
N3 Cd1 C24 105.71(8) .
N1 Cd1 C24 111.65(9) .
O3 Cd1 C24 27.01(8) .
O1 Cd1 C24 106.43(9) .
O2 Cd1 C24 124.39(9) .
O4 Cd1 C24 27.58(8) .
N3 Cd1 C11 114.28(9) .
N1 Cd1 C11 109.29(8) .
O3 Cd1 C11 133.93(8) .
O1 Cd1 C11 27.25(8) .
O2 Cd1 C11 26.88(8) .
O4 Cd1 C11 97.87(8) .
C24 Cd1 C11 118.67(8) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.353(4) .
C1 C2 1.399(4) .
C1 C4 1.499(4) .
C2 C3 1.423(4) .
C2 C2 1.470(6) 4
C3 N1 1.334(3) .
C3 C5 1.504(4) .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 N4 1.341(4) .
C6 C7 1.391(4) .
C6 C9 1.497(5) .
C7 C8 1.423(4) .
C7 C7 1.475(6) 5_765
C8 N3 1.341(4) .
C8 C10 1.489(4) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 O2 1.234(4) .
C11 O1 1.250(3) .
C11 C12 1.512(4) .
C11 Cd1 2.728(3) .
C12 C13 1.395(4) .
C12 C17 1.404(4) .
C13 C14 1.385(5) .
C13 H13 0.9300 .
C14 C15 1.382(5) .
C14 H14 0.9300 .
C15 C16 1.385(5) .
C15 H15 0.9300 .
C16 C17 1.389(4) .
C16 H16 0.9300 .
C17 C18 1.511(4) 5_655
C18 C19 1.397(4) .
C18 C23 1.406(4) .
C18 C17 1.511(4) 5_665
C19 C20 1.393(4) .
C19 H19 0.9300 .
C20 C21 1.371(4) .
C20 H20 0.9300 .
C21 C22 1.391(4) .
C21 H21 0.9300 .
C22 C23 1.395(4) .
C22 H22 0.9300 .
C23 C24 1.512(4) .
C24 O3 1.240(3) .
C24 O4 1.262(4) .
C24 Cd1 2.726(3) .
N1 N2 1.370(3) .
N1 Cd1 2.327(2) .
N2 H2N 0.79(3) .
N3 N4 1.370(3) .
N3 Cd1 2.287(2) .
N4 H4N 0.78(3) .
O1 Cd1 2.365(2) .
O2 Cd1 2.379(2) .
O3 Cd1 2.355(2) .
O4 Cd1 2.4079(19) .
