#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:03:29 +0100 (lun 21 de mar de 2016) $
#$Revision: 178766 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/20/4102040.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_4102040
loop_
_publ_author_name
'Chunying Duan'
'Meilin Wei'
'Dong Guo'
'Cheng He'
'Qingjin Meng'
_publ_section_title
;
 Crystal Structures and Properties of Large Protonated Water Clusters
 Encapsulated by Metal-Organic Frameworks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3321
_journal_page_last               3330
_journal_paper_doi               10.1021/ja907023c
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C144 H175 Co4 N36 O165 P3 W36'
_chemical_formula_weight         11997.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           204
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 2 2 3'
_symmetry_space_group_name_H-M   'I m -3'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.1603(12)
_cell_length_b                   23.1603(12)
_cell_length_c                   23.1603(12)
_cell_measurement_reflns_used    10860
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.035
_cell_measurement_theta_min      2.155
_cell_volume                     12423.2(11)
_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      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1068
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            37856
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    16.979
_exptl_absorpt_correction_T_max  0.1767
_exptl_absorpt_correction_T_min  0.1342
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    3.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10836
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.497
_refine_diff_density_min         -6.297
_refine_diff_density_rms         0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0516
_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)+(0.1800P)²+151.8000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2052
_refine_ls_wR_factor_ref         0.2115
_reflns_number_gt                2339
_reflns_number_total             2558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja907023c_si_001.cif
_cod_data_source_block           696018
_cod_database_code               4102040
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+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
W2 W 0.423485(19) 0.10865(2) 0.076887(19) 0.01852(15) Uani 1 1 d . . .
W1 W 0.34665(3) 0.0000 0.0000 0.0169(2) Uani 1 4 d S . .
W3 W 0.5000 0.0000 0.15426(4) 0.0222(2) Uani 1 4 d S . .
P1 P 0.5000 0.0000 0.0000 0.0097(14) Uani 1 8 d S . .
O1 O 0.5000 0.0412(8) 0.0553(7) 0.005(3) Uiso 0.50 2 d SP . 1
O1' O 0.4488(8) 0.0344(9) 0.0000 0.013(4) Uiso 0.50 2 d SP . 2
O2 O 0.2735(8) 0.0000 0.0000 0.044(6) Uani 1 4 d S . .
O3 O 0.3894(5) 0.1615(5) 0.1124(5) 0.049(3) Uani 1 1 d . . .
O4 O 0.5000 0.0000 0.2279(7) 0.028(4) Uani 1 4 d S . .
O5 O 0.3627(6) 0.0562(5) 0.0557(4) 0.051(3) Uani 1 1 d . . .
O6 O 0.4442(5) 0.0540(6) 0.1352(6) 0.075(4) Uani 1 1 d . . .
O7 O 0.4192(7) 0.1361(7) 0.0000 0.048(4) Uani 1 2 d S . .
O8 O 0.5000 0.1252(11) 0.0672(11) 0.024(5) Uiso 0.50 2 d SP . 1
O8' O 0.5000 0.1488(9) 0.0910(9) 0.014(4) Uiso 0.50 2 d SP . 2
Co1 Co 0.2500 0.2500 0.2500 0.0110(6) Uani 1 6 d S . .
O9 O 0.2759(4) 0.2088(3) 0.1758(3) 0.0181(16) Uani 1 1 d . . .
N1 N 0.2783(4) 0.1507(3) 0.1747(4) 0.0118(17) Uani 1 1 d . . .
C1 C 0.3157(4) 0.1233(4) 0.2117(5) 0.015(2) Uani 1 1 d . . .
H1A H 0.3389 0.1440 0.2372 0.018 Uiso 1 1 calc R . .
C2 C 0.3174(5) 0.0643(4) 0.2095(4) 0.014(2) Uani 1 1 d . . .
H2A H 0.3421 0.0446 0.2343 0.017 Uiso 1 1 calc R . .
C3 C 0.2825(4) 0.0321(4) 0.1704(4) 0.0108(19) Uani 1 1 d . . .
C4 C 0.2490(6) 0.0626(6) 0.1351(7) 0.035(3) Uani 1 1 d . . .
H4A H 0.2263 0.0432 0.1083 0.043 Uiso 1 1 calc R . .
C5 C 0.2468(5) 0.1231(5) 0.1367(5) 0.020(2) Uani 1 1 d . . .
H5A H 0.2233 0.1433 0.1112 0.024 Uiso 1 1 calc R . .
N2 N 0.5000 0.2389(8) 0.3285(11) 0.052(6) Uani 1 2 d S . .
C6 C 0.5000 0.1984(8) 0.2921(9) 0.029(4) Uani 1 2 d S . .
C7 C 0.5000 0.1543(14) 0.2492(11) 0.069(9) Uani 1 2 d S . .
H7C H 0.4616 0.1496 0.2343 0.083 Uiso 0.50 1 calc PR . .
H7A H 0.5127 0.1186 0.2661 0.083 Uiso 0.50 1 calc PR . .
H7B H 0.5257 0.1649 0.2185 0.083 Uiso 0.50 1 calc PR . .
O1W O 0.0000 -0.1644(11) -0.1021(16) 0.125(12) Uani 1 2 d S . .
O2W O 0.1006(6) 0.1006(6) 0.1006(6) 0.061(6) Uani 1 3 d S . .
O4W O 0.0000 0.0000 0.0000 0.14(4) Uani 1 24 d S . .
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'
Co Co 0.3494 0.9721 '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
_geom_angle_publ_flag
O3 W2 O8 111.3(9) . . ?
O3 W2 O7 101.1(7) . . ?
O8 W2 O7 82.3(9) . . ?
O3 W2 O6 104.8(7) . . ?
O8 W2 O6 89.0(8) . . ?
O7 W2 O6 154.1(8) . . ?
O3 W2 O5 104.1(6) . . ?
O8 W2 O5 144.2(9) . . ?
O7 W2 O5 86.2(5) . . ?
O6 W2 O5 86.9(5) . . ?
O3 W2 O8' 89.8(7) . . ?
O8 W2 O8' 22.4(8) . . ?
O7 W2 O8' 92.5(7) . . ?
O6 W2 O8' 88.3(7) . . ?
O5 W2 O8' 166.0(7) . . ?
O3 W2 O1 157.1(6) . . ?
O8 W2 O1 53.0(9) . . ?
O7 W2 O1 93.5(7) . . ?
O6 W2 O1 62.2(6) . . ?
O5 W2 O1 94.3(5) . . ?
O8' W2 O1 71.8(6) . . ?
O2 W1 O5 101.5(4) . 4 ?
O2 W1 O5 101.5(4) . . ?
O5 W1 O5 157.0(9) 4 . ?
O2 W1 O5 101.5(4) . 27 ?
O5 W1 O5 87.2(6) 4 27 ?
O5 W1 O5 88.2(7) . 27 ?
O2 W1 O5 101.5(4) . 26 ?
O5 W1 O5 88.2(7) 4 26 ?
O5 W1 O5 87.2(6) . 26 ?
O5 W1 O5 157.0(9) 27 26 ?
O2 W1 O1' 161.4(5) . . ?
O5 W1 O1' 91.9(6) 4 . ?
O5 W1 O1' 65.7(5) . . ?
O5 W1 O1' 91.9(6) 27 . ?
O5 W1 O1' 65.7(5) 26 . ?
O2 W1 O1' 161.4(5) . 27 ?
O5 W1 O1' 65.7(5) 4 27 ?
O5 W1 O1' 91.9(6) . 27 ?
O5 W1 O1' 65.7(5) 27 27 ?
O5 W1 O1' 91.9(6) 26 27 ?
O1' W1 O1' 37.3(9) . 27 ?
O4 W3 O6 103.8(5) . 2_655 ?
O4 W3 O6 103.8(5) . 27 ?
O6 W3 O6 88.4(7) 2_655 27 ?
O4 W3 O6 103.8(5) . 28_655 ?
O6 W3 O6 85.0(8) 2_655 28_655 ?
O6 W3 O6 152.4(10) 27 28_655 ?
O4 W3 O6 103.8(5) . . ?
O6 W3 O6 152.4(10) 2_655 . ?
O6 W3 O6 85.0(8) 27 . ?
O6 W3 O6 88.4(7) 28_655 . ?
O4 W3 O1 157.4(4) . 2_655 ?
O6 W3 O1 61.3(5) 2_655 2_655 ?
O6 W3 O1 61.3(5) 27 2_655 ?
O6 W3 O1 92.3(6) 28_655 2_655 ?
O6 W3 O1 92.3(6) . 2_655 ?
O4 W3 O1 157.4(4) . . ?
O6 W3 O1 92.3(6) 2_655 . ?
O6 W3 O1 92.3(6) 27 . ?
O6 W3 O1 61.3(5) 28_655 . ?
O6 W3 O1 61.3(5) . . ?
O1 W3 O1 45.3(8) 2_655 . ?
O1' P1 O1' 112.2(16) 27 25_655 ?
O1' P1 O1' 180.0(16) 27 3_655 ?
O1' P1 O1' 67.8(16) 25_655 3_655 ?
O1' P1 O1' 67.8(16) 27 . ?
O1' P1 O1' 180.0(16) 25_655 . ?
O1' P1 O1' 112.2(16) 3_655 . ?
O1' P1 O1 70.5(5) 27 25_655 ?
O1' P1 O1 70.5(5) 25_655 25_655 ?
O1' P1 O1 109.5(5) 3_655 25_655 ?
O1' P1 O1 109.5(5) . 25_655 ?
O1' P1 O1 109.5(5) 27 . ?
O1' P1 O1 109.5(5) 25_655 . ?
O1' P1 O1 70.5(5) 3_655 . ?
O1' P1 O1 70.5(5) . . ?
O1 P1 O1 180.0(13) 25_655 . ?
O1' P1 O1 70.5(5) 27 2_655 ?
O1' P1 O1 70.5(5) 25_655 2_655 ?
O1' P1 O1 109.5(5) 3_655 2_655 ?
O1' P1 O1 109.5(5) . 2_655 ?
O1 P1 O1 106.6(12) 25_655 2_655 ?
O1 P1 O1 73.4(12) . 2_655 ?
O1' P1 O1 109.5(5) 27 26 ?
O1' P1 O1 109.5(5) 25_655 26 ?
O1' P1 O1 70.5(5) 3_655 26 ?
O1' P1 O1 70.5(5) . 26 ?
O1 P1 O1 73.4(12) 25_655 26 ?
O1 P1 O1 106.6(12) . 26 ?
O1 P1 O1 180.0(13) 2_655 26 ?
P1 O1 W2 123.5(5) . 28_655 ?
P1 O1 W2 123.5(5) . . ?
W2 O1 W2 94.5(6) 28_655 . ?
P1 O1 W3 120.7(9) . . ?
W2 O1 W3 93.3(5) 28_655 . ?
W2 O1 W3 93.3(5) . . ?
P1 O1' O1' 56.1(8) . 27 ?
P1 O1' W1 127.4(11) . . ?
O1' O1' W1 71.4(5) 27 . ?
W1 O5 W2 139.6(7) . . ?
W3 O6 W2 142.3(8) . . ?
W2 O7 W2 140.3(10) 26 . ?
W2 O8 W2 151.8(15) 28_655 . ?
W2 O8' W2 121.8(11) 28_655 . ?
O9 Co1 O9 89.5(3) 9 . ?
O9 Co1 O9 90.5(3) 9 41 ?
O9 Co1 O9 90.5(3) . 41 ?
O9 Co1 O9 89.5(3) 9 5 ?
O9 Co1 O9 89.5(3) . 5 ?
O9 Co1 O9 180.0(4) 41 5 ?
O9 Co1 O9 180.0(2) 9 45 ?
O9 Co1 O9 90.5(3) . 45 ?
O9 Co1 O9 89.5(3) 41 45 ?
O9 Co1 O9 90.5(3) 5 45 ?
O9 Co1 O9 90.5(3) 9 37 ?
O9 Co1 O9 180.0(2) . 37 ?
O9 Co1 O9 89.5(3) 41 37 ?
O9 Co1 O9 90.5(3) 5 37 ?
O9 Co1 O9 89.5(3) 45 37 ?
N1 O9 Co1 119.5(6) . . ?
C5 N1 O9 118.4(9) . . ?
C5 N1 C1 123.0(9) . . ?
O9 N1 C1 118.5(9) . . ?
C2 C1 N1 117.2(10) . . ?
C1 C2 C3 122.0(9) . . ?
C4 C3 C2 116.3(10) . . ?
C4 C3 C3 122.1(7) . 27 ?
C2 C3 C3 121.5(5) . 27 ?
C3 C4 C5 122.4(12) . . ?
N1 C5 C4 119.0(11) . . ?
N2 C6 C7 178(2) . . ?
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
W2 O3 1.673(10) . ?
W2 O8 1.827(6) . ?
W2 O7 1.893(6) . ?
W2 O6 1.912(10) . ?
W2 O5 1.923(10) . ?
W2 O8' 2.028(11) . ?
W2 O1 2.414(12) . ?
W1 O2 1.693(17) . ?
W1 O5 1.869(9) 4 ?
W1 O5 1.869(9) . ?
W1 O5 1.869(9) 27 ?
W1 O5 1.869(9) 26 ?
W1 O1' 2.50(2) . ?
W1 O1' 2.50(2) 27 ?
W3 O4 1.705(16) . ?
W3 O6 1.852(12) 2_655 ?
W3 O6 1.852(12) 27 ?
W3 O6 1.852(12) 28_655 ?
W3 O6 1.852(12) . ?
W3 O1 2.482(17) 2_655 ?
W3 O1 2.482(17) . ?
P1 O1' 1.43(2) 27 ?
P1 O1' 1.43(2) 25_655 ?
P1 O1' 1.43(2) 3_655 ?
P1 O1' 1.43(2) . ?
P1 O1 1.598(18) 25_655 ?
P1 O1 1.598(18) . ?
P1 O1 1.598(18) 2_655 ?
P1 O1 1.598(18) 26 ?
O1 W2 2.414(12) 28_655 ?
O1' O1' 1.60(4) 27 ?
O7 W2 1.893(6) 26 ?
O8 W2 1.827(6) 28_655 ?
O8' W2 2.028(11) 28_655 ?
Co1 O9 2.054(8) 9 ?
Co1 O9 2.054(8) . ?
Co1 O9 2.054(8) 41 ?
Co1 O9 2.054(8) 5 ?
Co1 O9 2.054(8) 45 ?
Co1 O9 2.054(8) 37 ?
O9 N1 1.348(11) . ?
N1 C5 1.310(15) . ?
N1 C1 1.373(13) . ?
C1 C2 1.368(14) . ?
C2 C3 1.426(14) . ?
C3 C4 1.330(17) . ?
C3 C3 1.487(18) 27 ?
C4 C5 1.402(18) . ?
N2 C6 1.26(3) . ?
C6 C7 1.42(4) . ?
