#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:46:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179393 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/90/4329054.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_4329054
loop_
_publ_author_name
'Qiuxia Han'
'Lejie Zhang'
'Cheng He'
'Jiangyang Niu'
'Chunying Duan'
_publ_section_title
;
 Metal-Organic Frameworks with Phosphotungstate Incorporated for
 Hydrolytic Cleavage of a DNA-Model Phosphodiester
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5118
_journal_page_last               5127
_journal_paper_doi               10.1021/ic202685e
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C40 H32 N8 O56 P W12 Yb2'
_chemical_formula_weight         4103.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 105.990(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.232(6)
_cell_length_b                   17.416(5)
_cell_length_c                   11.738(3)
_cell_measurement_reflns_used    2849
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.036
_cell_measurement_theta_min      2.338
_cell_volume                     3779.5(19)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9475
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    20.758
_exptl_absorpt_correction_T_max  0.1035
_exptl_absorpt_correction_T_min  0.0680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            clorless
_exptl_crystal_density_diffrn    3.606
_exptl_crystal_description       block
_exptl_crystal_F_000             3638
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.518
_refine_diff_density_min         -5.803
_refine_diff_density_rms         0.501
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3416
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.1037
_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)+(0.0998P)²+2506.0967P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2796
_refine_ls_wR_factor_ref         0.2822
_reflns_number_gt                3115
_reflns_number_total             3416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202685e_si_005.cif
_cod_data_source_block           1
_cod_original_cell_volume        3779.4(19)
_cod_database_code               4329054
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_disorder_group
W1 W 0.64345(9) -0.39843(11) -0.06265(14) 0.0410(5) Uani 1 1 d . .
W2 W 0.67208(12) -0.5000 0.20685(19) 0.0334(6) Uani 1 2 d S .
W3 W 0.52840(11) -0.39833(10) 0.26890(13) 0.0434(6) Uani 1 1 d . .
W4 W 0.5000 -0.29686(14) 0.0000 0.0597(9) Uani 1 2 d S .
P1 P 0.5000 -0.5000 0.0000 0.027(4) Uani 1 4 d S .
Yb1 Yb 0.95988(11) -0.5000 0.62561(18) 0.0205(5) Uani 1 2 d S .
O1 O 0.715(2) -0.349(3) -0.086(4) 0.084(12) Uani 1 1 d U .
O2 O 0.685(2) -0.4243(17) 0.100(2) 0.053(9) Uani 1 1 d . .
O3 O 0.595(2) -0.319(3) -0.012(4) 0.088(12) Uani 1 1 d U .
O4 O 0.577(3) -0.393(3) -0.209(5) 0.105(14) Uani 1 1 d U .
O5 O 0.662(3) -0.5000 -0.099(4) 0.062(13) Uani 1 2 d S .
O6 O 0.751(2) -0.5000 0.306(4) 0.048(10) Uani 1 2 d SU .
O7 O 0.627(2) -0.424(3) 0.276(4) 0.086(12) Uani 1 1 d U .
O8 O 0.5425(16) -0.3491(19) 0.397(3) 0.053(8) Uani 1 1 d . .
O9 O 0.518(3) -0.5000 0.324(5) 0.063 Uiso 1 2 d S .
O10 O 0.533(2) -0.317(2) 0.166(4) 0.073(10) Uani 1 1 d U .
O11 O 0.5000 -0.202(3) 0.0000 0.057(12) Uani 1 2 d SU .
O12 O 0.579(6) -0.5000 0.017(10) 0.07(2) Uani 0.50 2 d SPU 1
O13 O 0.546(4) -0.5000 0.136(6) 0.033(15) Uani 0.50 2 d SPU 2
O14 O 0.529(2) -0.426(2) -0.062(4) 0.020(9) Uani 0.50 1 d PU 2
O15 O 1.0608(17) -0.5000 0.569(3) 0.040(10) Uani 1 2 d S .
O21 O 0.8797(15) -0.5981(16) 0.559(2) 0.038(6) Uani 1 1 d U .
O22 O 0.5179(17) -0.9112(18) 0.762(3) 0.054(9) Uani 1 1 d . .
O1W O 0.895(2) -0.5000 0.767(3) 0.038(9) Uani 1 2 d S .
O2W O 0.616(3) -0.5000 0.589(7) 0.10(2) Uani 1 2 d S .
O3W O 0.756(2) -0.5000 0.733(3) 0.038 Uiso 1 2 d S .
C1 C 0.762(2) -0.632(3) 0.539(4) 0.043(9) Uani 1 1 d U .
H1A H 0.7490 -0.6029 0.4700 0.051 Uiso 1 1 calc R .
C2 C 0.712(2) -0.669(2) 0.572(4) 0.043(10) Uani 1 1 d . .
H2A H 0.6632 -0.6603 0.5319 0.052 Uiso 1 1 calc R .
C3 C 0.7301(18) -0.7190(19) 0.665(3) 0.024(7) Uani 1 1 d U .
C4 C 0.7994(19) -0.724(2) 0.730(3) 0.029(7) Uani 1 1 d U .
H4A H 0.8123 -0.7553 0.7968 0.034 Uiso 1 1 calc R .
C5 C 0.8529(18) -0.680(3) 0.696(3) 0.037(10) Uani 1 1 d . .
H5A H 0.9011 -0.6822 0.7403 0.044 Uiso 1 1 calc R .
C6 C 0.6714(19) -0.764(2) 0.696(3) 0.028(7) Uani 1 1 d U .
C7 C 0.600(2) -0.762(2) 0.633(3) 0.036(8) Uani 1 1 d U .
H7A H 0.5858 -0.7258 0.5729 0.043 Uiso 1 1 calc R .
C8 C 0.550(2) -0.810(2) 0.653(3) 0.033(8) Uani 1 1 d U .
H8A H 0.5019 -0.8083 0.6073 0.040 Uiso 1 1 calc R .
C9 C 0.686(3) -0.814(3) 0.791(5) 0.063(13) Uani 1 1 d U .
H9A H 0.7324 -0.8132 0.8426 0.075 Uiso 1 1 calc R .
C10 C 0.636(3) -0.865(4) 0.817(6) 0.072(14) Uani 1 1 d U .
H10A H 0.6478 -0.8981 0.8809 0.087 Uiso 1 1 calc R .
N1 N 0.8332(15) -0.6343(16) 0.599(2) 0.024(6) Uani 1 1 d U .
N2 N 0.5712(16) -0.8614(17) 0.744(3) 0.027(6) Uani 1 1 d U .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
O1 W1 O4 102(2) . .
O1 W1 O3 100(2) . .
O4 W1 O3 89(2) . .
O1 W1 O5 103(2) . .
O4 W1 O5 88(2) . .
O3 W1 O5 157(2) . .
O1 W1 O2 98.5(19) . .
O4 W1 O2 160(2) . .
O3 W1 O2 88.0(17) . .
O5 W1 O2 87.1(17) . .
O1 W1 O14 159.3(19) . .
O4 W1 O14 65(2) . .
O3 W1 O14 64.9(18) . .
O5 W1 O14 93(2) . .
O2 W1 O14 95.3(16) . .
O1 W1 O12 158(3) . .
O4 W1 O12 96(3) . .
O3 W1 O12 94(2) . .
O5 W1 O12 64(2) . .
O2 W1 O12 65(3) . .
O14 W1 O12 43(3) . .
O6 W2 O7 98.1(18) . 6_545
O6 W2 O7 98.1(18) . .
O7 W2 O7 89(3) 6_545 .
O6 W2 O2 101.8(15) . 6_545
O7 W2 O2 87.6(17) 6_545 6_545
O7 W2 O2 160.1(18) . 6_545
O6 W2 O2 101.8(15) . .
O7 W2 O2 160.1(18) 6_545 .
O7 W2 O2 87.6(17) . .
O2 W2 O2 88.8(18) 6_545 .
O6 W2 O13 157(2) . .
O7 W2 O13 66.3(18) 6_545 .
O7 W2 O13 66.3(18) . .
O2 W2 O13 94.6(17) 6_545 .
O2 W2 O13 94.6(17) . .
O6 W2 O12 162(3) . .
O7 W2 O12 95(2) 6_545 .
O7 W2 O12 95(2) . .
O2 W2 O12 66(2) 6_545 .
O2 W2 O12 66(2) . .
O13 W2 O12 41(3) . .
O8 W3 O10 99.9(18) . .
O8 W3 O9 100.0(19) . .
O10 W3 O9 160.2(19) . .
O8 W3 O7 99.6(17) . .
O10 W3 O7 89.1(18) . .
O9 W3 O7 88(2) . .
O8 W3 O4 101.0(19) . 2_655
O10 W3 O4 88(2) . 2_655
O9 W3 O4 88(2) . 2_655
O7 W3 O4 159(2) . 2_655
O8 W3 O14 155.7(15) . 2_655
O10 W3 O14 65.7(16) . 2_655
O9 W3 O14 95.5(18) . 2_655
O7 W3 O14 99.6(17) . 2_655
O4 W3 O14 60.6(19) 2_655 2_655
O8 W3 O13 156.9(19) . .
O10 W3 O13 95.3(18) . .
O9 W3 O13 65.9(19) . .
O7 W3 O13 63(2) . .
O4 W3 O13 97(2) 2_655 .
O14 W3 O13 47.5(19) 2_655 .
O11 W4 O3 101.6(14) . 2_655
O11 W4 O3 101.6(14) . .
O3 W4 O3 157(3) 2_655 .
O11 W4 O10 100.8(12) . .
O3 W4 O10 86.8(18) 2_655 .
O3 W4 O10 88.9(18) . .
O11 W4 O10 100.8(12) . 2_655
O3 W4 O10 88.9(18) 2_655 2_655
O3 W4 O10 86.8(18) . 2_655
O10 W4 O10 158(2) . 2_655
O11 W4 O14 155.3(10) . 2_655
O3 W4 O14 59.9(17) 2_655 2_655
O3 W4 O14 97.9(18) . 2_655
O10 W4 O14 64.2(16) . 2_655
O10 W4 O14 95.4(16) 2_655 2_655
O11 W4 O14 155.3(10) . .
O3 W4 O14 97.9(18) 2_655 .
O3 W4 O14 59.9(17) . .
O10 W4 O14 95.4(16) . .
O10 W4 O14 64.2(16) 2_655 .
O14 W4 O14 49(2) 2_655 .
O12 P1 O12 180(9) 5_645 .
O12 P1 O13 114(5) 5_645 .
O12 P1 O13 66(5) . .
O12 P1 O13 66(5) 5_645 5_645
O12 P1 O13 114(5) . 5_645
O13 P1 O13 180.000(12) . 5_645
O12 P1 O14 67(3) 5_645 2_655
O12 P1 O14 113(3) . 2_655
O13 P1 O14 74(2) . 2_655
O13 P1 O14 106(2) 5_645 2_655
O12 P1 O14 67(3) 5_645 5_645
O12 P1 O14 113(3) . 5_645
O13 P1 O14 74(2) . 5_645
O13 P1 O14 106(2) 5_645 5_645
O14 P1 O14 103(3) 2_655 5_645
O12 P1 O14 113(3) 5_645 .
O12 P1 O14 67(3) . .
O13 P1 O14 106(2) . .
O13 P1 O14 74(2) 5_645 .
O14 P1 O14 77(3) 2_655 .
O14 P1 O14 180(3) 5_645 .
O12 P1 O14 113(3) 5_645 6_545
O12 P1 O14 67(3) . 6_545
O13 P1 O14 106(2) . 6_545
O13 P1 O14 74(2) 5_645 6_545
O14 P1 O14 180(3) 2_655 6_545
O14 P1 O14 77(3) 5_645 6_545
O14 P1 O14 103(3) . 6_545
O15 Yb1 O15 67.3(14) 5_746 .
O15 Yb1 O22 129.8(9) 5_746 3
O15 Yb1 O22 84.9(10) . 3
O15 Yb1 O22 129.8(9) 5_746 8_535
O15 Yb1 O22 84.9(10) . 8_535
O22 Yb1 O22 85.1(19) 3 8_535
O15 Yb1 O21 74.6(9) 5_746 .
O15 Yb1 O21 117.4(8) . .
O22 Yb1 O21 153.8(10) 3 .
O22 Yb1 O21 83.6(12) 8_535 .
O15 Yb1 O21 74.6(9) 5_746 6_545
O15 Yb1 O21 117.4(8) . 6_545
O22 Yb1 O21 83.6(12) 3 6_545
O22 Yb1 O21 153.8(10) 8_535 6_545
O21 Yb1 O21 96.5(14) . 6_545
O15 Yb1 O1W 139.1(13) 5_746 .
O15 Yb1 O1W 153.6(14) . .
O22 Yb1 O1W 75.8(10) 3 .
O22 Yb1 O1W 75.8(10) 8_535 .
O21 Yb1 O1W 78.5(10) . .
O21 Yb1 O1W 78.5(10) 6_545 .
O15 Yb1 Yb1 33.7(8) 5_746 5_746
O15 Yb1 Yb1 33.6(9) . 5_746
O22 Yb1 Yb1 109.3(7) 3 5_746
O22 Yb1 Yb1 109.3(7) 8_535 5_746
O21 Yb1 Yb1 96.7(7) . 5_746
O21 Yb1 Yb1 96.7(7) 6_545 5_746
O1W Yb1 Yb1 172.7(10) . 5_746
W2 O2 W1 137.2(19) . .
W1 O3 W4 139(3) . .
W1 O4 W3 136(3) . 2_655
W1 O5 W1 141(3) 6_545 .
W2 O7 W3 135(3) . .
W3 O9 W3 135(3) . 6_545
W3 O10 W4 138(2) . .
P1 O12 W2 126(6) . .
P1 O12 W1 123(4) . .
W2 O12 W1 92(3) . .
P1 O12 W1 123(4) . 6_545
W2 O12 W1 92(3) . 6_545
W1 O12 W1 91(4) . 6_545
P1 O13 W2 126(4) . .
P1 O13 W3 120(2) . 6_545
W2 O13 W3 95(2) . 6_545
P1 O13 W3 120(2) . .
W2 O13 W3 95(2) . .
W3 O13 W3 93(3) 6_545 .
P1 O14 W1 128(2) . .
P1 O14 W3 119(2) . 2_655
W1 O14 W3 97.6(16) . 2_655
P1 O14 W4 117(2) . .
W1 O14 W4 96.3(16) . .
W3 O14 W4 92.4(15) 2_655 .
Yb1 O15 Yb1 112.7(14) 5_746 .
N1 O21 Yb1 135(2) . .
N2 O22 Yb1 123(2) . 3_445
C2 C1 N1 124(4) . .
C2 C1 H1A 118.0 . .
N1 C1 H1A 118.0 . .
C1 C2 C3 120(4) . .
C1 C2 H2A 120.2 . .
C3 C2 H2A 120.2 . .
C4 C3 C2 120(3) . .
C4 C3 C6 121(3) . .
C2 C3 C6 119(3) . .
C3 C4 C5 119(3) . .
C3 C4 H4A 120.5 . .
C5 C4 H4A 120.5 . .
N1 C5 C4 120(3) . .
N1 C5 H5A 120.2 . .
C4 C5 H5A 120.2 . .
C7 C6 C9 114(4) . .
C7 C6 C3 124(3) . .
C9 C6 C3 122(4) . .
C8 C7 C6 123(4) . .
C8 C7 H7A 118.4 . .
C6 C7 H7A 118.4 . .
C7 C8 N2 118(4) . .
C7 C8 H8A 121.2 . .
N2 C8 H8A 121.2 . .
C6 C9 C10 125(5) . .
C6 C9 H9A 117.6 . .
C10 C9 H9A 117.6 . .
N2 C10 C9 115(5) . .
N2 C10 H10A 122.5 . .
C9 C10 H10A 122.5 . .
O21 N1 C1 120(3) . .
O21 N1 C5 122(3) . .
C1 N1 C5 118(3) . .
C10 N2 C8 125(4) . .
C10 N2 O22 119(4) . .
C8 N2 O22 116(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.71(4) .
W1 O4 1.85(5) .
W1 O3 1.86(5) .
W1 O5 1.875(17) .
W1 O2 1.91(2) .
W1 O14 2.26(4) .
W1 O12 2.48(8) .
W2 O6 1.63(4) .
W2 O7 1.88(5) 6_545
W2 O7 1.88(5) .
W2 O2 1.88(3) 6_545
W2 O2 1.88(3) .
W2 O13 2.33(7) .
W2 O12 2.44(11) .
W3 O8 1.69(3) .
W3 O10 1.88(4) .
W3 O9 1.91(2) .
W3 O7 1.93(5) .
W3 O4 1.95(5) 2_655
W3 O14 2.42(4) 2_655
W3 O13 2.45(5) .
W4 O11 1.66(5) .
W4 O3 1.90(5) 2_655
W4 O3 1.90(5) .
W4 O10 1.90(4) .
W4 O10 1.90(4) 2_655
W4 O14 2.47(4) 2_655
W4 O14 2.47(4) .
P1 O12 1.48(11) 5_645
P1 O12 1.48(11) .
P1 O13 1.60(7) .
P1 O13 1.60(7) 5_645
P1 O14 1.66(4) 2_655
P1 O14 1.66(4) 5_645
P1 O14 1.66(4) .
P1 O14 1.66(4) 6_545
Yb1 O15 2.21(4) 5_746
Yb1 O15 2.22(3) .
Yb1 O22 2.29(3) 3
Yb1 O22 2.29(3) 8_535
Yb1 O21 2.29(3) .
Yb1 O21 2.29(3) 6_545
Yb1 O1W 2.34(3) .
Yb1 Yb1 3.686(4) 5_746
O4 W3 1.95(5) 2_655
O5 W1 1.875(17) 6_545
O9 W3 1.91(2) 6_545
O12 W1 2.48(8) 6_545
O13 W3 2.45(5) 6_545
O14 W3 2.42(4) 2_655
O15 Yb1 2.21(4) 5_746
O21 N1 1.29(4) .
O22 N2 1.40(4) .
O22 Yb1 2.29(3) 3_445
C1 C2 1.31(6) .
C1 N1 1.35(5) .
C1 H1A 0.9300 .
C2 C3 1.37(5) .
C2 H2A 0.9300 .
C3 C4 1.35(5) .
C3 C6 1.50(5) .
C4 C5 1.43(5) .
C4 H4A 0.9300 .
C5 N1 1.35(5) .
C5 H5A 0.9300 .
C6 C7 1.37(5) .
C6 C9 1.38(6) .
C7 C8 1.36(5) .
C7 H7A 0.9300 .
C8 N2 1.36(5) .
C8 H8A 0.9300 .
C9 C10 1.40(8) .
C9 H9A 0.9300 .
C10 N2 1.30(7) .
C10 H10A 0.9300 .
