#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:25:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180434 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/03/7210347.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_7210347
loop_
_publ_author_name
'Hu, Dong-Hua'
'Sun, Chun-Yi'
'Liu, Fu-Hong'
'Qin, Chao'
'Wang, Xin-Long'
'Su, Zhong-Min'
_publ_section_title
;
 A series of coordination complexes based on unsymmetrical
 multicarboxylate ligands: syntheses, structures and properties
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              6769
_journal_paper_doi               10.1039/c3ce40782a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C68 H86 Cd6 N24 O41'
_chemical_formula_weight         2570.01
_chemical_name_systematic
; 
 ? 
;
_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                 110.792(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.532(3)
_cell_length_b                   19.713(3)
_cell_length_c                   15.214(3)
_cell_measurement_reflns_used    10366
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      1.74
_cell_volume                     4354.9(14)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_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  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10366
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_T_max  0.7171
_exptl_absorpt_correction_T_min  0.6889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2556
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.700
_refine_diff_density_min         -1.302
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         3821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0553P)²+114.7413P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1660
_reflns_number_gt                2878
_reflns_number_total             3821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40782a.txt
_cod_data_source_block           www
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7210347
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
C1 C 0.1824(7) 0.1341(6) 0.4656(7) 0.044(3) Uani 1 1 d .
C2 C 0.2203(7) 0.1779(7) 0.4140(8) 0.052(3) Uani 1 1 d .
H2A H 0.1822 0.2074 0.3695 0.062 Uiso 1 1 calc R
C3 C 0.3125(7) 0.1764(6) 0.4301(7) 0.046(3) Uani 1 1 d .
C4 C 0.3694(7) 0.1331(6) 0.4987(7) 0.041(3) Uani 1 1 d .
H4A H 0.4325 0.1325 0.5108 0.049 Uiso 1 1 calc R
C5 C 0.3323(6) 0.0911(5) 0.5485(6) 0.031(2) Uani 1 1 d .
C6 C 0.2397(6) 0.0917(5) 0.5328(7) 0.034(2) Uani 1 1 d .
H6A H 0.2157 0.0635 0.5676 0.041 Uiso 1 1 calc R
C7 C 0.0803(8) 0.1329(9) 0.4438(8) 0.067(5) Uani 1 1 d .
C8 C 0.3953(6) 0.0436(5) 0.6201(7) 0.034(2) Uani 1 1 d .
C9 C 0.4423(8) 0.2225(6) 0.3985(10) 0.056(3) Uani 1 1 d .
H9A H 0.4734 0.2280 0.4665 0.068 Uiso 1 1 calc R
C10 C 0.4619(10) 0.2848(7) 0.3496(11) 0.074(4) Uani 1 1 d .
H10A H 0.4393 0.3245 0.3710 0.111 Uiso 1 1 calc R
H10B H 0.4315 0.2802 0.2829 0.111 Uiso 1 1 calc R
H10C H 0.5270 0.2889 0.3642 0.111 Uiso 1 1 calc R
C11 C 0.4801(7) 0.1576(6) 0.3673(8) 0.041(3) Uani 1 1 d .
C12 C -0.2453(7) 0.0806(5) 0.5118(7) 0.034(2) Uani 1 1 d .
H12A H -0.2942 0.0977 0.4614 0.041 Uiso 1 1 calc R
C13 C -0.1147(7) 0.0494(6) 0.6019(8) 0.044(3) Uani 1 1 d .
H13A H -0.0520 0.0396 0.6246 0.053 Uiso 1 1 calc R
C16 C -0.3324(7) 0.0586(6) 0.6173(8) 0.041(3) Uani 1 1 d .
H16A H -0.3411 0.0144 0.6409 0.049 Uiso 1 1 calc R
H16B H -0.3865 0.0687 0.5627 0.049 Uiso 1 1 calc R
C17 C -0.3216(7) 0.1119(6) 0.6926(8) 0.047(3) Uani 1 1 d .
H17A H -0.3752 0.1104 0.7112 0.056 Uiso 1 1 calc R
H17B H -0.2682 0.1007 0.7473 0.056 Uiso 1 1 calc R
C14 C -0.2522(7) 0.2628(6) 0.6223(9) 0.049(3) Uani 1 1 d .
H14A H -0.2108 0.2904 0.6075 0.059 Uiso 1 1 calc R
C15 C -0.3688(7) 0.2323(6) 0.6494(8) 0.044(3) Uani 1 1 d .
H15A H -0.4252 0.2311 0.6578 0.053 Uiso 1 1 calc R
Cd1 Cd -0.10628(5) 0.10747(4) 0.39765(5) 0.0353(2) Uani 1 1 d .
Cd2 Cd 0.5000 -0.04727(6) 0.7500 0.0346(3) Uani 1 2 d S
N1 N -0.1588(6) 0.0766(5) 0.5153(6) 0.039(2) Uani 1 1 d .
N2 N -0.1675(6) 0.0382(5) 0.6503(6) 0.043(2) Uani 1 1 d .
N3 N -0.2515(5) 0.0571(4) 0.5902(5) 0.0305(18) Uani 1 1 d .
N4 N -0.3112(6) 0.1799(5) 0.6631(6) 0.041(2) Uani 1 1 d .
N5 N -0.2355(6) 0.1992(5) 0.6444(7) 0.046(2) Uani 1 1 d .
N6 N -0.3345(6) 0.2859(5) 0.6223(6) 0.043(2) Uani 1 1 d .
O1 O 0.0286(6) 0.1665(9) 0.3764(7) 0.128(6) Uani 1 1 d .
O2 O 0.0479(5) 0.0961(5) 0.4924(7) 0.063(2) Uani 1 1 d .
O3 O 0.3604(4) 0.0058(4) 0.6664(5) 0.0402(17) Uani 1 1 d .
O4 O 0.4785(4) 0.0418(5) 0.6327(5) 0.056(2) Uani 1 1 d .
O5 O 0.3436(6) 0.2191(5) 0.3781(6) 0.064(3) Uani 1 1 d .
O6 O 0.4234(5) 0.1222(5) 0.3063(5) 0.055(2) Uani 1 1 d .
O7 O 0.5613(5) 0.1476(4) 0.4034(6) 0.059(2) Uani 1 1 d .
O1W O -0.0974(6) -0.0082(6) 0.3582(7) 0.086(3) Uani 1 1 d .
O2W O -0.2494(5) 0.0795(4) 0.2855(5) 0.052(2) Uani 1 1 d .
O3W O -0.0726(13) 0.0774(13) 0.2611(13) 0.203(9) Uani 1 1 d .
O4W O -0.5000 0.1944(18) 0.7500 0.141(17) Uani 0.50 2 d SP
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'
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'
H H 0.0000 0.0000 '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
C6 C1 C2 119.5(10) . .
C6 C1 C7 120.6(11) . .
C2 C1 C7 119.8(11) . .
C3 C2 C1 120.0(10) . .
C3 C2 H2A 120.0 . .
C1 C2 H2A 120.0 . .
O5 C3 C2 116.8(10) . .
O5 C3 C4 123.7(10) . .
C2 C3 C4 119.6(11) . .
C5 C4 C3 120.1(9) . .
C5 C4 H4A 120.0 . .
C3 C4 H4A 120.0 . .
C6 C5 C4 121.1(9) . .
C6 C5 C8 120.2(9) . .
C4 C5 C8 118.7(8) . .
C5 C6 C1 119.7(10) . .
C5 C6 H6A 120.1 . .
C1 C6 H6A 120.1 . .
O1 C7 O2 120.9(12) . .
O1 C7 C1 119.8(15) . .
O2 C7 C1 119.3(11) . .
O4 C8 O3 121.6(9) . .
O4 C8 C5 120.3(9) . .
O3 C8 C5 118.0(8) . .
O4 C8 Cd2 63.2(6) . .
O3 C8 Cd2 58.4(5) . .
C5 C8 Cd2 176.3(7) . .
O5 C9 C10 108.2(10) . .
O5 C9 C11 112.5(10) . .
C10 C9 C11 110.7(10) . .
O5 C9 H9A 108.5 . .
C10 C9 H9A 108.5 . .
C11 C9 H9A 108.5 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O7 C11 O6 126.9(11) . .
O7 C11 C9 116.5(11) . .
O6 C11 C9 116.6(10) . .
N3 C12 N1 110.0(9) . .
N3 C12 H12A 125.0 . .
N1 C12 H12A 125.0 . .
N2 C13 N1 114.3(9) . .
N2 C13 H13A 122.8 . .
N1 C13 H13A 122.8 . .
N3 C16 C17 110.6(8) . .
N3 C16 H16A 109.5 . .
C17 C16 H16A 109.5 . .
N3 C16 H16B 109.5 . .
C17 C16 H16B 109.5 . .
H16A C16 H16B 108.1 . .
N4 C17 C16 113.8(9) . .
N4 C17 H17A 108.8 . .
C16 C17 H17A 108.8 . .
N4 C17 H17B 108.8 . .
C16 C17 H17B 108.8 . .
H17A C17 H17B 107.7 . .
N5 C14 N6 115.2(10) . .
N5 C14 H14A 122.4 . .
N6 C14 H14A 122.4 . .
N6 C15 N4 110.4(9) . .
N6 C15 H15A 124.8 . .
N4 C15 H15A 124.8 . .
N6 Cd1 N1 96.4(3) 7_456 .
N6 Cd1 O2 116.8(3) 7_456 .
N1 Cd1 O2 93.7(3) . .
N6 Cd1 O2W 83.5(3) 7_456 .
N1 Cd1 O2W 89.8(3) . .
O2 Cd1 O2W 158.8(3) . .
N6 Cd1 O1W 155.8(3) 7_456 .
N1 Cd1 O1W 90.6(4) . .
O2 Cd1 O1W 85.7(3) . .
O2W Cd1 O1W 73.4(3) . .
N6 Cd1 O3W 108.5(7) 7_456 .
N1 Cd1 O3W 149.2(6) . .
O2 Cd1 O3W 91.1(5) . .
O2W Cd1 O3W 75.6(5) . .
O1W Cd1 O3W 59.5(7) . .
N6 Cd1 O1 82.6(4) 7_456 .
N1 Cd1 O1 139.9(3) . .
O2 Cd1 O1 53.3(3) . .
O2W Cd1 O1 129.4(3) . .
O1W Cd1 O1 106.6(4) . .
O3W Cd1 O1 63.5(6) . .
O6 Cd2 O6 97.9(5) 6_556 5_656
O6 Cd2 O3 127.0(3) 6_556 2_656
O6 Cd2 O3 89.3(3) 5_656 2_656
O6 Cd2 O3 89.3(3) 6_556 .
O6 Cd2 O3 127.0(3) 5_656 .
O3 Cd2 O3 126.8(3) 2_656 .
O6 Cd2 O4 98.5(3) 6_556 2_656
O6 Cd2 O4 142.9(3) 5_656 2_656
O3 Cd2 O4 54.5(2) 2_656 2_656
O3 Cd2 O4 86.3(3) . 2_656
O6 Cd2 O4 142.9(2) 6_556 .
O6 Cd2 O4 98.5(3) 5_656 .
O3 Cd2 O4 86.3(3) 2_656 .
O3 Cd2 O4 54.5(2) . .
O4 Cd2 O4 87.9(4) 2_656 .
O6 Cd2 C8 114.4(3) 6_556 2_656
O6 Cd2 C8 116.5(3) 5_656 2_656
O3 Cd2 C8 27.6(2) 2_656 2_656
O3 Cd2 C8 107.4(3) . 2_656
O4 Cd2 C8 26.9(2) 2_656 2_656
O4 Cd2 C8 87.1(3) . 2_656
O6 Cd2 C8 116.5(3) 6_556 .
O6 Cd2 C8 114.4(3) 5_656 .
O3 Cd2 C8 107.4(3) 2_656 .
O3 Cd2 C8 27.6(2) . .
O4 Cd2 C8 87.1(3) 2_656 .
O4 Cd2 C8 26.9(2) . .
C8 Cd2 C8 98.2(4) 2_656 .
C12 N1 C13 102.5(8) . .
C12 N1 Cd1 126.0(7) . .
C13 N1 Cd1 131.5(7) . .
C13 N2 N3 102.9(8) . .
C12 N3 N2 110.2(8) . .
C12 N3 C16 126.7(8) . .
N2 N3 C16 122.5(8) . .
C15 N4 N5 109.4(9) . .
C15 N4 C17 128.8(9) . .
N5 N4 C17 121.8(8) . .
C14 N5 N4 102.5(8) . .
C15 N6 C14 102.5(9) . .
C15 N6 Cd1 126.6(7) . 7_456
C14 N6 Cd1 130.3(8) . 7_456
C7 O1 Cd1 88.4(11) . .
C7 O2 Cd1 96.8(7) . .
C8 O3 Cd2 93.9(5) . .
C8 O4 Cd2 89.9(6) . .
C3 O5 C9 118.1(9) . .
C11 O6 Cd2 108.9(6) . 5_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.375(14) .
C1 C2 1.426(16) .
C1 C7 1.500(15) .
C2 C3 1.366(14) .
C2 H2A 0.9300 .
C3 O5 1.356(13) .
C3 C4 1.393(14) .
C4 C5 1.379(14) .
C4 H4A 0.9300 .
C5 C6 1.373(12) .
C5 C8 1.505(13) .
C6 H6A 0.9300 .
C7 O1 1.245(16) .
C7 O2 1.261(17) .
C8 O4 1.237(11) .
C8 O3 1.271(12) .
C8 Cd2 2.734(10) .
C9 O5 1.454(14) .
C9 C10 1.520(17) .
C9 C11 1.550(16) .
C9 H9A 0.9800 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 O7 1.200(12) .
C11 O6 1.243(13) .
C12 N3 1.315(12) .
C12 N1 1.328(12) .
C12 H12A 0.9300 .
C13 N2 1.301(13) .
C13 N1 1.361(13) .
C13 H13A 0.9300 .
C16 N3 1.455(12) .
C16 C17 1.519(15) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 N4 1.440(14) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C14 N5 1.299(14) .
C14 N6 1.357(13) .
C14 H14A 0.9300 .
C15 N6 1.313(14) .
C15 N4 1.333(13) .
C15 H15A 0.9300 .
Cd1 N6 2.271(9) 7_456
Cd1 N1 2.297(8) .
Cd1 O2 2.327(7) .
Cd1 O2W 2.338(7) .
Cd1 O1W 2.374(11) .
Cd1 O3W 2.390(18) .
Cd1 O1 2.515(13) .
Cd2 O6 2.248(7) 6_556
Cd2 O6 2.248(7) 5_656
Cd2 O3 2.336(7) 2_656
Cd2 O3 2.336(6) .
Cd2 O4 2.441(8) 2_656
Cd2 O4 2.441(8) .
Cd2 C8 2.734(10) 2_656
N2 N3 1.353(11) .
N4 N5 1.360(11) .
N6 Cd1 2.271(9) 7_456
O6 Cd2 2.248(7) 5_656
