#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:49:15 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180357 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/26/7202670.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_7202670
loop_
_publ_author_name
'Duan, Xianying'
'Li, Yizhi'
'Su, Yang'
'Zang, Shuangquan'
'Zhu, Chengjian'
'Meng, Qingjin'
_publ_section_title
;
 Syntheses and solid state structures of hybrid d10 metal--organic
 frameworks based on methylenediisophthalic acid (H4MDIP)
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              758
_journal_paper_doi               10.1039/b618613k
_journal_volume                  9
_journal_year                    2007
_chemical_formula_moiety         'C21 H32 Cd2 N4 O12, 2(H2 O)'
_chemical_formula_sum            'C21 H36 Cd2 N4 O14'
_chemical_formula_weight         793.34
_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                 102.4630(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.277(3)
_cell_length_b                   9.8838(18)
_cell_length_c                   15.724(3)
_cell_measurement_reflns_used    3560
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.075
_cell_measurement_theta_min      2.283
_cell_volume                     2773.5(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'phi and omega 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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7205
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    1.609
_exptl_absorpt_correction_T_max  0.7605
_exptl_absorpt_correction_T_min  0.6987
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    multi-scan
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0481
_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)+(0.0700P)²+1.9900P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1140
_reflns_number_gt                2138
_reflns_number_total             2713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b618613k.txt
_cod_data_source_block           cd
_cod_original_cell_volume        2773.7(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7202670
#BEGIN Tags that were not found in dictionaries:
_refine_diff_density             0.479
#END Tags that were not found in dictionaries
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
C1 C 0.9094(3) 0.5650(6) 0.9266(4) 0.0420(13) Uani 1 1 d . . .
C2 C 0.9588(3) 0.6649(6) 0.9588(4) 0.0426(13) Uani 1 1 d . . .
H2 H 0.9495 0.7192 1.0036 0.051 Uiso 1 1 calc R . .
C3 C 1.0226(3) 0.6883(5) 0.9269(4) 0.0404(13) Uani 1 1 d . . .
C4 C 1.0363(3) 0.6023(5) 0.8592(3) 0.0372(12) Uani 1 1 d . . .
H4 H 1.0792 0.6149 0.8374 0.045 Uiso 1 1 calc R . .
C5 C 0.9863(3) 0.5000(5) 0.8254(4) 0.0388(13) Uani 1 1 d . . .
C6 C 0.9240(3) 0.4799(6) 0.8602(4) 0.0407(12) Uani 1 1 d . . .
H6 H 0.8913 0.4094 0.8396 0.049 Uiso 1 1 calc R . .
C7 C 0.8414(3) 0.5448(5) 0.9614(3) 0.0345(12) Uani 1 1 d . . .
C8 C 1.0788(3) 0.7985(6) 0.9593(4) 0.0437(13) Uani 1 1 d . . .
C9 C 1.0000 0.4135(8) 0.7500 0.0312(15) Uani 1 2 d S . .
H9A H 0.9569 0.3558 0.7296 0.037 Uiso 0.50 1 calc PR . .
H9B H 1.0431 0.3558 0.7704 0.037 Uiso 0.50 1 calc PR . .
C10 C 0.7386(4) 0.4085(6) 1.2010(4) 0.0485(14) Uani 1 1 d . . .
H10A H 0.7737 0.3707 1.2505 0.058 Uiso 1 1 calc R . .
H10B H 0.6883 0.3960 1.2106 0.058 Uiso 1 1 calc R . .
C11 C 0.7545(3) 0.5614(6) 1.1930(4) 0.0362(12) Uani 1 1 d . . .
H11A H 0.7475 0.6070 1.2452 0.043 Uiso 1 1 calc R . .
H11B H 0.8064 0.5730 1.1893 0.043 Uiso 1 1 calc R . .
Cd1 Cd 0.70184(2) 0.47772(4) 1.00260(3) 0.03748(16) Uani 1 1 d . . .
N1 N 0.7460(2) 0.3371(4) 1.1200(2) 0.0290(9) Uani 1 1 d . . .
H1A H 0.7194 0.2598 1.1142 0.035 Uiso 1 1 calc R . .
H1B H 0.7944 0.3163 1.1225 0.035 Uiso 1 1 calc R . .
N2 N 0.7051(2) 0.6272(5) 1.1150(3) 0.0437(11) Uani 1 1 d . . .
H2A H 0.7243 0.7071 1.1033 0.052 Uiso 1 1 calc R . .
H2B H 0.6587 0.6410 1.1242 0.052 Uiso 1 1 calc R . .
O1 O 0.8244(2) 0.6222(4) 1.0148(3) 0.0434(10) Uani 1 1 d . . .
O2 O 0.7995(2) 0.4427(4) 0.9340(2) 0.0379(9) Uani 1 1 d . . .
O3 O 1.07501(18) 0.8565(4) 1.0267(2) 0.0345(8) Uani 1 1 d . . .
O4 O 1.12629(19) 0.8251(4) 0.9149(2) 0.0335(8) Uani 1 1 d . . .
O5 O 0.6492(2) 0.6405(4) 0.9014(2) 0.0374(8) Uani 1 1 d . . .
H5A H 0.6033 0.6220 0.8815 0.056 Uiso 1 1 d R . .
H5B H 0.6528 0.7178 0.9256 0.056 Uiso 1 1 d R . .
O6 O 0.4969(2) 0.5986(4) 0.8432(2) 0.0464(10) Uani 1 1 d . . .
H6D H 0.5437 0.6112 0.8611 0.056 Uiso 1 1 d R . .
H6C H 0.4755 0.6027 0.8861 0.070 Uiso 1 1 d R . .
O7 O 0.0836(2) 0.8655(4) 0.7374(2) 0.0380(8) Uani 1 1 d . . .
H7B H 0.0727 0.8982 0.7831 0.057 Uiso 1 1 d R . .
H7C H 0.0791 0.9266 0.6985 0.057 Uiso 1 1 d R . .
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
C2 C1 C6 119.4(6) . . ?
C2 C1 C7 120.4(5) . . ?
C6 C1 C7 120.2(5) . . ?
C1 C2 C3 122.1(6) . . ?
C1 C2 H2 119.0 . . ?
C3 C2 H2 119.0 . . ?
C2 C3 C4 117.9(5) . . ?
C2 C3 C8 124.4(5) . . ?
C4 C3 C8 117.7(5) . . ?
C5 C4 C3 120.8(5) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C6 C5 C4 119.0(5) . . ?
C6 C5 C9 121.0(5) . . ?
C4 C5 C9 120.0(5) . . ?
C5 C6 C1 120.8(5) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
O1 C7 O2 120.1(4) . . ?
O1 C7 C1 121.9(5) . . ?
O2 C7 C1 118.1(5) . . ?
O3 C8 O4 124.2(5) . . ?
O3 C8 C3 118.0(5) . . ?
O4 C8 C3 117.9(5) . . ?
C5 C9 C5 111.8(6) . 2_756 ?
C5 C9 H9A 109.2 . . ?
C5 C9 H9A 109.2 2_756 . ?
C5 C9 H9B 109.2 . . ?
C5 C9 H9B 109.2 2_756 . ?
H9A C9 H9B 107.9 . . ?
N1 C10 C11 109.8(5) . . ?
N1 C10 H10A 109.7 . . ?
C11 C10 H10A 109.7 . . ?
N1 C10 H10B 109.7 . . ?
C11 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
N2 C11 C10 113.5(5) . . ?
N2 C11 H11A 108.9 . . ?
C10 C11 H11A 108.9 . . ?
N2 C11 H11B 108.9 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
O4 Cd1 N2 142.97(15) 3_445 . ?
O4 Cd1 O2 92.67(13) 3_445 . ?
N2 Cd1 O2 124.34(15) . . ?
O4 Cd1 N1 98.38(14) 3_445 . ?
N2 Cd1 N1 79.96(15) . . ?
O2 Cd1 N1 96.40(14) . . ?
O4 Cd1 O5 86.40(13) 3_445 . ?
N2 Cd1 O5 91.14(15) . . ?
O2 Cd1 O5 91.77(13) . . ?
N1 Cd1 O5 170.31(13) . . ?
O4 Cd1 O1 142.59(12) 3_445 . ?
N2 Cd1 O1 73.39(15) . . ?
O2 Cd1 O1 51.76(12) . . ?
N1 Cd1 O1 97.05(14) . . ?
O5 Cd1 O1 83.91(14) . . ?
C10 N1 Cd1 108.5(3) . . ?
C10 N1 H1A 110.0 . . ?
Cd1 N1 H1A 110.0 . . ?
C10 N1 H1B 110.0 . . ?
Cd1 N1 H1B 110.0 . . ?
H1A N1 H1B 108.4 . . ?
C11 N2 Cd1 105.1(3) . . ?
C11 N2 H2A 110.7 . . ?
Cd1 N2 H2A 110.7 . . ?
C11 N2 H2B 110.7 . . ?
Cd1 N2 H2B 110.7 . . ?
H2A N2 H2B 108.8 . . ?
C7 O1 Cd1 87.1(3) . . ?
C7 O2 Cd1 101.0(3) . . ?
C8 O4 Cd1 101.7(3) . 3 ?
Cd1 O5 H5A 109.4 . . ?
Cd1 O5 H5B 109.5 . . ?
H5A O5 H5B 109.5 . . ?
H6D O6 H6C 109.5 . . ?
H7B O7 H7C 109.5 . . ?
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
C1 C2 1.360(8) . ?
C1 C6 1.411(8) . ?
C1 C7 1.475(8) . ?
C2 C3 1.384(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.426(8) . ?
C3 C8 1.508(7) . ?
C4 C5 1.389(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.379(8) . ?
C5 C9 1.526(7) . ?
C6 H6 0.9300 . ?
C7 O1 1.224(6) . ?
C7 O2 1.283(6) . ?
C8 O3 1.221(7) . ?
C8 O4 1.252(7) . ?
C9 C5 1.526(7) 2_756 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N1 1.488(7) . ?
C10 C11 1.549(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.505(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
Cd1 O4 2.294(3) 3_445 ?
Cd1 N2 2.294(5) . ?
Cd1 O2 2.303(3) . ?
Cd1 N1 2.313(4) . ?
Cd1 O5 2.321(4) . ?
Cd1 O1 2.628(4) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
O4 Cd1 2.294(3) 3 ?
O5 H5A 0.8501 . ?
O5 H5B 0.8499 . ?
O6 H6D 0.8501 . ?
O6 H6C 0.8499 . ?
O7 H7B 0.8499 . ?
O7 H7C 0.8501 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O2 0.90 2.14 2.960(6) 150.7 7_657
N2 H2A O1 0.90 2.52 3.181(7) 130.2 7_667
O5 H5B O1 0.85 1.84 2.682(5) 171.2 7_667
O6 H6C O3 0.85 1.86 2.696(5) 169.7 7_667
N1 H1B O4 0.90 2.18 2.978(5) 146.8 5_767
N2 H2B O7 0.90 2.47 3.238(6) 143.2 8_566
O5 H5A O6 0.85 1.92 2.768(5) 173.4 .
O6 H6D O5 0.85 1.92 2.768(5) 179.7 .
O7 H7B O4 0.85 2.21 2.761(5) 122.0 1_455
O7 H7C O6 0.85 2.20 2.876(6) 136.0 4_556
