#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:28:07 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179580 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/45/4504572.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_4504572
loop_
_publ_author_name
'Zhang, Guoqi'
'Yang, Guoqiang'
'Ma, Jin Shi'
_publ_section_title
;
 Versatile Framework Solids Constructed from Divalent Transition Metals
 and Citric Acid:  Syntheses, Crystal Structures, and Thermal
 Behaviors
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              375
_journal_paper_doi               10.1021/cg0503245
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C12 H22 Cd3 N0 O20'
_chemical_formula_weight         823.50
_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                 109.09(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.550(3)
_cell_length_b                   10.257(2)
_cell_length_c                   18.015(4)
_cell_measurement_reflns_used    20515
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.32
_cell_volume                     2191.5(9)
_computing_cell_refinement       'Rapid Auto(Rigaku 2001)'
_computing_data_collection       'Rapid Auto(Rigaku 2001)'
_computing_data_reduction        'Rapid Auto(Rigaku 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Raxis Rapid IP Area Detector'
_diffrn_measurement_method       'ω Oscillation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20515
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    2.983
_exptl_absorpt_correction_T_max  0.7567
_exptl_absorpt_correction_T_min  0.4544
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Abscor
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0289P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0477
_reflns_number_gt                4466
_reflns_number_total             5016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0503245si20050906_104340.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2191.5(8)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4504572
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
Cd1 Cd 0.337140(15) 0.457984(16) 0.363310(10) 0.02130(5) Uani 1 1 d .
Cd2 Cd 0.329591(14) 0.562423(16) 0.113518(9) 0.01827(5) Uani 1 1 d .
Cd3 Cd 0.347136(14) 0.249975(17) -0.076004(9) 0.02066(5) Uani 1 1 d .
O4 O 0.19227(14) 0.70944(17) 0.13394(11) 0.0268(4) Uani 1 1 d .
O1W O 0.12478(19) -0.0290(2) -0.21368(14) 0.0350(5) Uani 1 1 d .
H2W H 0.095(3) 0.019(3) -0.251(2) 0.033(9) Uiso 1 1 d .
H1W H 0.094(3) -0.065(4) -0.199(2) 0.051(14) Uiso 1 1 d .
O5 O 0.02770(16) 0.80168(18) 0.11098(13) 0.0359(5) Uani 1 1 d .
O1 O 0.15378(14) 0.44323(17) 0.07127(9) 0.0212(3) Uani 1 1 d .
H1A H 0.184(3) 0.363(4) 0.074(2) 0.056(11) Uiso 1 1 d .
O2 O 0.29134(14) 0.46506(18) 0.21904(10) 0.0250(4) Uani 1 1 d .
O3 O 0.15708(15) 0.43994(17) 0.27117(9) 0.0242(3) Uani 1 1 d .
O6 O 0.17019(18) 0.19014(18) 0.12052(14) 0.0403(5) Uani 1 1 d .
O7 O 0.01623(19) 0.10188(19) 0.12881(13) 0.0412(5) Uani 1 1 d .
O15 O 0.2825(3) 0.4348(3) 0.47005(15) 0.0559(7) Uani 1 1 d .
H15B H 0.298(3) 0.494(4) 0.4982(19) 0.036(9) Uiso 1 1 d .
H15A H 0.304(4) 0.364(5) 0.491(2) 0.063(13) Uiso 1 1 d .
O16 O 0.43803(17) 0.7214(2) 0.18987(13) 0.0311(4) Uani 1 1 d .
H16B H 0.415(3) 0.774(4) 0.201(2) 0.046(12) Uiso 1 1 d .
H16A H 0.477(4) 0.752(4) 0.167(2) 0.060(13) Uiso 1 1 d .
O9 O 0.35069(14) 0.35232(18) 0.04404(10) 0.0264(4) Uani 1 1 d .
O10 O 0.48109(16) 0.41500(17) 0.15257(10) 0.0273(4) Uani 1 1 d .
O8 O 0.44239(15) 0.12887(18) 0.03680(9) 0.0218(3) Uani 1 1 d .
H8A H 0.462(3) 0.065(3) 0.0446(19) 0.030(9) Uiso 1 1 d .
O11 O 0.52642(14) 0.33476(17) -0.04049(10) 0.0252(4) Uani 1 1 d .
O12 O 0.71157(14) 0.33840(18) 0.00536(10) 0.0266(4) Uani 1 1 d .
O13 O 0.56436(19) -0.05921(18) 0.11925(10) 0.0351(5) Uani 1 1 d .
O14 O 0.63478(17) -0.04020(16) 0.24879(9) 0.0287(4) Uani 1 1 d .
O17 O 0.2423(2) 0.4376(2) -0.10837(13) 0.0374(5) Uani 1 1 d .
H17B H 0.215(3) 0.462(3) -0.155(2) 0.037(9) Uiso 1 1 d .
H17A H 0.237(4) 0.488(4) -0.082(3) 0.069(15) Uiso 1 1 d .
O18 O 0.19120(16) 0.1268(2) -0.08756(12) 0.0291(4) Uani 1 1 d .
H18B H 0.141(4) 0.159(5) -0.083(3) 0.077(16) Uiso 1 1 d .
H18A H 0.182(4) 0.083(5) -0.125(3) 0.082(16) Uiso 1 1 d .
O19 O 0.2983(2) 0.2684(2) -0.21044(11) 0.0345(5) Uani 1 1 d .
H19B H 0.318(3) 0.324(3) -0.232(2) 0.038(10) Uiso 1 1 d .
H19A H 0.320(3) 0.197(4) -0.232(2) 0.064(12) Uiso 1 1 d .
C4 C 0.0885(2) 0.7008(2) 0.12080(13) 0.0197(4) Uani 1 1 d .
C3 C 0.0290(2) 0.5728(2) 0.11736(13) 0.0203(4) Uani 1 1 d .
H3A H -0.0290 0.5666 0.0664 0.024 Uiso 1 1 calc R
H3B H -0.0089 0.5749 0.1564 0.024 Uiso 1 1 calc R
C1 C 0.09949(19) 0.4481(2) 0.13016(13) 0.0172(4) Uani 1 1 d .
C2 C 0.18958(19) 0.4505(2) 0.21227(13) 0.0179(4) Uani 1 1 d .
C5 C 0.0191(2) 0.3329(2) 0.12096(14) 0.0227(5) Uani 1 1 d .
H5A H -0.0145 0.3375 0.1623 0.027 Uiso 1 1 calc R
H5B H -0.0412 0.3417 0.0712 0.027 Uiso 1 1 calc R
C6 C 0.0722(2) 0.2000(2) 0.12367(14) 0.0247(5) Uani 1 1 d .
C8 C 0.44203(19) 0.3339(2) 0.09828(13) 0.0186(4) Uani 1 1 d .
C7 C 0.50900(18) 0.2089(2) 0.09941(12) 0.0152(4) Uani 1 1 d .
C9 C 0.6216(2) 0.2424(2) 0.08837(13) 0.0214(5) Uani 1 1 d .
H9B H 0.6634 0.2984 0.1314 0.026 Uiso 1 1 calc R
H9A H 0.6644 0.1624 0.0927 0.026 Uiso 1 1 calc R
C10 C 0.6167(2) 0.3090(2) 0.01182(13) 0.0188(4) Uani 1 1 d .
C11 C 0.5282(2) 0.1388(2) 0.17813(12) 0.0186(4) Uani 1 1 d .
H11A H 0.5768 0.1923 0.2200 0.022 Uiso 1 1 calc R
H11B H 0.4564 0.1304 0.1871 0.022 Uiso 1 1 calc R
C12 C 0.5809(2) 0.0040(2) 0.18253(12) 0.0202(4) Uani 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
O15 Cd1 O5 99.60(10) . 2_545
O15 Cd1 O7 118.01(10) . 2
O5 Cd1 O7 84.97(7) 2_545 2
O15 Cd1 O3 96.00(10) . .
O5 Cd1 O3 125.08(7) 2_545 .
O7 Cd1 O3 131.03(7) 2 .
O15 Cd1 O6 88.10(9) . 2
O5 Cd1 O6 136.95(7) 2_545 2
O7 Cd1 O6 54.91(7) 2 2
O3 Cd1 O6 95.64(7) . 2
O15 Cd1 O2 150.27(9) . .
O5 Cd1 O2 97.85(7) 2_545 .
O7 Cd1 O2 87.30(7) 2 .
O3 Cd1 O2 54.29(6) . .
O6 Cd1 O2 95.35(7) 2 .
O15 Cd1 O4 78.12(8) . 2_545
O5 Cd1 O4 53.11(6) 2_545 2_545
O7 Cd1 O4 137.84(6) 2 2_545
O3 Cd1 O4 79.85(6) . 2_545
O6 Cd1 O4 164.88(6) 2 2_545
O2 Cd1 O4 93.65(6) . 2_545
O15 Cd1 C6 105.01(9) . 2
O5 Cd1 C6 111.41(7) 2_545 2
O7 Cd1 C6 27.37(7) 2 2
O3 Cd1 C6 114.59(7) . 2
O6 Cd1 C6 27.57(7) 2 2
O2 Cd1 C6 90.62(7) . 2
O4 Cd1 C6 164.37(7) 2_545 2
O15 Cd1 C2 123.18(10) . .
O5 Cd1 C2 113.53(7) 2_545 .
O7 Cd1 C2 109.98(8) 2 .
O3 Cd1 C2 27.19(6) . .
O6 Cd1 C2 96.18(7) 2 .
O2 Cd1 C2 27.10(6) . .
O4 Cd1 C2 86.39(6) 2_545 .
C6 Cd1 C2 103.86(7) 2 .
O12 Cd2 O16 98.95(8) 3_665 .
O12 Cd2 O2 156.34(6) 3_665 .
O16 Cd2 O2 93.20(7) . .
O12 Cd2 O10 118.85(6) 3_665 .
O16 Cd2 O10 90.84(7) . .
O2 Cd2 O10 80.94(6) . .
O12 Cd2 O4 84.84(7) 3_665 .
O16 Cd2 O4 77.02(7) . .
O2 Cd2 O4 78.18(6) . .
O10 Cd2 O4 155.10(6) . .
O12 Cd2 O1 91.54(7) 3_665 .
O16 Cd2 O1 148.93(7) . .
O2 Cd2 O1 68.29(6) . .
O10 Cd2 O1 109.55(6) . .
O4 Cd2 O1 74.90(6) . .
O12 Cd2 O9 86.78(6) 3_665 .
O16 Cd2 O9 139.90(7) . .
O2 Cd2 O9 96.91(6) . .
O10 Cd2 O9 53.07(6) . .
O4 Cd2 O9 143.06(6) . .
O1 Cd2 O9 69.42(6) . .
O18 Cd3 O11 165.28(7) . .
O18 Cd3 O17 92.18(8) . .
O11 Cd3 O17 100.42(8) . .
O18 Cd3 O19 91.38(8) . .
O11 Cd3 O19 99.28(8) . .
O17 Cd3 O19 74.40(8) . .
O18 Cd3 O8 87.98(7) . .
O11 Cd3 O8 77.54(6) . .
O17 Cd3 O8 138.63(7) . .
O19 Cd3 O8 146.98(7) . .
O18 Cd3 O9 95.02(7) . .
O11 Cd3 O9 81.67(6) . .
O17 Cd3 O9 72.63(7) . .
O19 Cd3 O9 146.59(7) . .
O8 Cd3 O9 66.16(6) . .
O18 Cd3 O13 89.62(8) . 3_655
O11 Cd3 O13 83.60(7) . 3_655
O17 Cd3 O13 148.64(7) . 3_655
O19 Cd3 O13 74.26(7) . 3_655
O8 Cd3 O13 72.72(6) . 3_655
O9 Cd3 O13 138.38(6) . 3_655
C4 O4 Cd2 132.95(16) . .
C4 O4 Cd1 85.79(13) . 2
Cd2 O4 Cd1 137.43(7) . 2
C4 O5 Cd1 99.97(15) . 2
C1 O1 Cd2 110.74(13) . .
C2 O2 Cd2 116.56(14) . .
C2 O2 Cd1 88.74(13) . .
Cd2 O2 Cd1 146.14(8) . .
C2 O3 Cd1 95.01(14) . .
C6 O6 Cd1 89.84(15) . 2_545
C6 O7 Cd1 93.60(16) . 2_545
C8 O9 Cd3 112.37(14) . .
C8 O9 Cd2 87.70(14) . .
Cd3 O9 Cd2 147.25(8) . .
C8 O10 Cd2 96.98(15) . .
C7 O8 Cd3 112.41(13) . .
C10 O11 Cd3 134.22(15) . .
C10 O12 Cd2 105.17(14) . 3_665
C12 O13 Cd3 136.25(16) . 3_655
O4 C4 O5 120.9(2) . .
O4 C4 C3 122.9(2) . .
O5 C4 C3 116.2(2) . .
C4 C3 C1 118.02(19) . .
O1 C1 C5 110.39(18) . .
O1 C1 C3 107.97(18) . .
C5 C1 C3 107.59(18) . .
O1 C1 C2 109.46(18) . .
C5 C1 C2 111.56(18) . .
C3 C1 C2 109.79(18) . .
O2 C2 O3 122.0(2) . .
O2 C2 C1 120.04(19) . .
O3 C2 C1 118.0(2) . .
O2 C2 Cd1 64.16(12) . .
O3 C2 Cd1 57.80(12) . .
C1 C2 Cd1 175.62(15) . .
C6 C5 C1 115.3(2) . .
O7 C6 O6 121.5(2) . .
O7 C6 C5 118.5(2) . .
O6 C6 C5 120.0(2) . .
O7 C6 Cd1 59.02(14) . 2_545
O6 C6 Cd1 62.59(13) . 2_545
C5 C6 Cd1 176.24(17) . 2_545
O9 C8 O10 122.2(2) . .
O9 C8 C7 119.7(2) . .
O10 C8 C7 118.2(2) . .
O8 C7 C8 107.16(18) . .
O8 C7 C9 110.77(17) . .
C8 C7 C9 109.71(18) . .
O8 C7 C11 109.58(18) . .
C8 C7 C11 108.90(17) . .
C9 C7 C11 110.63(18) . .
C10 C9 C7 116.96(19) . .
O11 C10 O12 122.0(2) . .
O11 C10 C9 122.6(2) . .
O12 C10 C9 115.4(2) . .
C12 C11 C7 114.01(17) . .
O14 C12 O13 123.5(2) . .
O14 C12 C11 118.00(19) . .
O13 C12 C11 118.47(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O15 2.255(2) .
Cd1 O5 2.2690(19) 2_545
Cd1 O7 2.327(2) 2
Cd1 O3 2.3330(19) .
Cd1 O6 2.404(2) 2
Cd1 O2 2.4725(17) .
Cd1 O4 2.5787(18) 2_545
Cd1 C6 2.708(3) 2
Cd1 C2 2.747(2) .
Cd2 O12 2.2725(17) 3_665
Cd2 O16 2.276(2) .
Cd2 O2 2.3321(16) .
Cd2 O10 2.3498(18) .
Cd2 O4 2.4070(17) .
Cd2 O1 2.4174(18) .
Cd2 O9 2.5490(18) .
Cd3 O18 2.281(2) .
Cd3 O11 2.2992(18) .
Cd3 O17 2.296(2) .
Cd3 O19 2.304(2) .
Cd3 O8 2.3479(18) .
Cd3 O9 2.3913(17) .
Cd3 O13 2.4970(18) 3_655
O4 C4 1.248(3) .
O4 Cd1 2.5787(18) 2
O5 C4 1.263(3) .
O5 Cd1 2.2690(19) 2
O1 C1 1.437(3) .
O2 C2 1.252(3) .
O3 C2 1.260(3) .
O6 C6 1.253(3) .
O6 Cd1 2.404(2) 2_545
O7 C6 1.248(3) .
O7 Cd1 2.327(2) 2_545
O9 C8 1.254(3) .
O10 C8 1.255(3) .
O8 C7 1.424(3) .
O11 C10 1.242(3) .
O12 C10 1.270(3) .
O12 Cd2 2.2725(17) 3_665
O13 C12 1.268(3) .
O13 Cd3 2.4970(18) 3_655
O14 C12 1.249(3) .
C4 C3 1.502(3) .
C3 C1 1.529(3) .
C1 C5 1.527(3) .
C1 C2 1.541(3) .
C5 C6 1.511(3) .
C6 Cd1 2.708(3) 2_545
C8 C7 1.530(3) .
C7 C9 1.529(3) .
C7 C11 1.537(3) .
C9 C10 1.522(3) .
C11 C12 1.523(3) .
