A High Stable Polyoxometalate-Based Metal-Organic Framework with ABW Zeolite-Like Structure
Su, Zhong-Min; Li, Xiao-Xin; Shen, Feng-Cui; Liu, Jiang; Li, Shun-Li; Dong, Long-Zhang; Fu, Qiang; Lan, Ya-Qian; Chem. Commun.  (2017) –; doi:10.1039/C7CC05552H

data_7120552
_publ_section_title
;
 A High Stable Polyoxometalate-Based Metal-Organic Framework with ABW
 Zeolite-Like Structure
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC05552H
_journal_year                    2017
_chemical_formula_moiety
'0.25(C104 H80 Mo96 N36 O336 P8 Zn32), 3(H2 O)'
_chemical_formula_sum            'C26 H26 Mo24 N9 O87 P2 Zn8'
_chemical_formula_weight         4744.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-09 deposited with the CCDC.
2017-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.1749(16)
_cell_length_b                   38.738(3)
_cell_length_c                   52.010(4)
_cell_measurement_reflns_used    9200
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      24.925
_cell_measurement_theta_min      2.575
_cell_volume                     40648(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.71
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'BrukerAXS area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            109435
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.119
_diffrn_reflns_theta_max         25.119
_diffrn_reflns_theta_min         2.165
_exptl_absorpt_coefficient_mu    2.421
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1091 before and 0.0569 after correction.
The Ratio of minimum to maximum transmission is 0.6362.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull dark black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       block
_exptl_crystal_F_000             17752
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.31
_platon_squeeze_details
;
TITL mo_lixx170I b a mm     R = 0.08
CELL   20.1749   38.7380   52.0100     90.00     90.00     90.00
SPGR Ibam
C101 0.061 0.359-0.002 !       2.42 eA-3
C102 0.517 0.172 0.001 !       2.09 eA-3
C103 0.500 1.000 0.168 !       1.89 eA-3
Q104 0.357 0.376 0.167 !       1.75 eA-3
C105 0.500 0.499 0.121 !       1.68 eA-3
C106 0.591 0.298 0.061 !       1.64 eA-3
C107 0.939 0.617-0.001 !       1.64 eA-3
Q108 0.890 0.101 0.069 !       1.61 eA-3
C109 0.523 0.759 0.204 !       1.60 eA-3
C110 0.500 0.501 0.078 !       1.57 eA-3
C111 0.976 0.102 0.001 !       1.52 eA-3
C112 0.921 0.040 0.414 !       1.47 eA-3
C113 0.894 0.078 0.001 !       1.45 eA-3
C114 0.925 0.852 0.000 !       1.44 eA-3
C115 0.913 0.102 0.001 !       1.41 eA-3
Q116 0.190 0.789 0.152 !       1.40 eA-3
C117 0.550 0.985 0.149 !       1.39 eA-3
C118 0.472 0.234 0.001 !       1.39 eA-3
C119 0.964 0.281 0.206 !       1.38 eA-3
C120 0.095 0.950 0.430 !       1.38 eA-3
C121 0.543 0.727 0.433 !       1.35 eA-3
C122 0.999 0.015 0.100 !       1.33 eA-3
C123 0.055 0.203-0.002 !       1.31 eA-3
C124 0.845 0.976 0.168 !       1.30 eA-3
C125 0.949 0.040 0.421 !       1.28 eA-3
C126 0.628 0.961 0.123 !       1.28 eA-3
C127 0.937 0.460 0.142 !       1.28 eA-3
C128 0.888 0.556 0.396 !       1.28 eA-3
Q129 0.606 0.423 0.363 !       1.25 eA-3
C130 0.023 0.164-0.001 !       1.24 eA-3
C131 0.382 0.573 0.078 !       1.24 eA-3
C132 0.486 0.359 0.002 !       1.23 eA-3
C133 0.364 0.055 0.093 !       1.22 eA-3
C134 0.124 0.554 0.125 !       1.22 eA-3
Q135 0.854 0.835 0.450 !       1.21 eA-3
C136 0.379 0.655 0.075 !       1.20 eA-3
Q137 0.808 0.680 0.000 !       1.20 eA-3
C138 0.298 0.716 0.249 !       1.19 eA-3
Q139 0.576 0.330 0.384 !       1.19 eA-3
C140 0.018 0.963 0.408 !       1.18 eA-3
C141 0.860 0.063 0.437 !       1.18 eA-3
C142 0.485 0.255 0.308 !       1.17 eA-3
Q143 0.849 0.156 0.000 !       1.16 eA-3
C144 0.380 0.552 0.488 !       1.16 eA-3
C145 0.269 0.227 0.001 !       1.16 eA-3
C146 0.955 0.016 0.378 !       1.15 eA-3
C147 0.918 0.361 0.485 !       1.14 eA-3
C148 0.871 0.359 0.091 !       1.14 eA-3
C149 0.136 0.024 0.158 !       1.14 eA-3
C150 0.376 0.086 0.089 !       1.14 eA-3
C151 0.900 0.047 0.004 !       1.14 eA-3
C152 0.577 0.468 0.154 !       1.13 eA-3
C153 0.051 0.547 0.062 !       1.13 eA-3
C154 0.436 0.073 0.062 !       1.12 eA-3
C155 0.970 0.493 0.347 !       1.12 eA-3
C156 0.023 0.032 0.119 !       1.12 eA-3
C157 0.529 0.039 0.184 !       1.11 eA-3
C158 0.607 0.897 0.074 !       1.11 eA-3
C159 0.687 0.961 0.142 !       1.11 eA-3
C160 0.628 0.132 0.419 !       1.11 eA-3
C161 0.250 0.250 0.250 !       1.09 eA-3
C162 0.395 0.679 0.056 !       1.09 eA-3
C163 0.437 0.977 0.448 !       1.09 eA-3
C164 0.494 0.726 0.298 !       1.08 eA-3
C165 0.662 0.149 0.436 !       1.07 eA-3
C166 0.409 0.076 0.097 !       1.07 eA-3
C167 0.575 0.375-0.002 !       1.06 eA-3
C168 0.949 0.038 0.394 !       1.06 eA-3
C169 0.502 0.719 0.001 !       1.05 eA-3
C170 0.563 0.493 0.139 !       1.05 eA-3
C171 0.822 0.805 0.246 !       1.04 eA-3
C172 0.121 0.531 0.149 !       1.02 eA-3
C173 1.000 0.502 0.457 !       1.02 eA-3
C174 0.842 0.258 0.000 !       1.02 eA-3
C175 0.404 0.695 0.024 !       1.02 eA-3
C176 0.095 0.986 0.335 !       1.01 eA-3
C177 0.142 0.400 0.396 !       1.01 eA-3
C178 0.966 0.595 0.010 !       1.01 eA-3
C179 0.465 0.502 0.057 !       1.01 eA-3
C180 0.527 0.745 0.289 !       1.01 eA-3
C181 0.287 0.047 0.147 !       0.99 eA-3
C182 0.616 0.078 0.426 !       0.99 eA-3
C183 0.550 0.781 0.000 !       0.98 eA-3
C184 0.126 0.954 0.417 !       0.98 eA-3
Q185 0.310 0.850 0.176 !       0.98 eA-3
C186 0.673 0.938 0.073 !       0.97 eA-3
C187 0.605 0.398 0.078 !       0.97 eA-3
C188 0.395 0.602 0.922 !       0.97 eA-3
C189 0.395 0.601 0.078 !       0.97 eA-3
C190 0.182 0.787 0.266 !       0.96 eA-3
C191 0.210 0.251 0.241 !       0.95 eA-3
C192 0.149 0.617 0.065 !       0.95 eA-3
Q193 0.170 0.367-0.001 !       0.95 eA-3
C194 0.954 0.991 0.371 !       0.95 eA-3
C195 0.971 0.225 0.465 !       0.95 eA-3
C196 0.691 0.763 0.017 !       0.94 eA-3
Q197 0.522 0.554 0.390 !       0.94 eA-3
C198 0.086 0.382 0.418 !       0.94 eA-3
C199 0.516 0.920 0.286 !       0.93 eA-3
;
_refine_diff_density_max         1.357
_refine_diff_density_min         -1.338
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         18225
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+355.2773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13180
_reflns_number_total             18225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc05552h2.cif
_cod_data_source_block           mo_lixx170303_1_0m_sq
_cod_original_cell_volume        40648(6)
_cod_database_code               7120552
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H,H) groups, All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1W-H1WA
 0.8 with sigma of 0.05
 H1WB-O1W
 0.8 with sigma of 0.02
 N3-H1WB
 2 with sigma of 0.02
 O36-H36
 0.85 with sigma of 0.01
 O17-H17
 0.85 with sigma of 0.01
 H2W-O2W
 0.8 with sigma of 0.02
 H2W-O35_$1
 1.86 with sigma of 0.02
 Mo11-H36
 2.224216 with sigma of 0.02
 Mo10-H36
 2.598454 with sigma of 0.02
 Mo5-H17
 2.229708 with sigma of 0.02
 Mo6-H17
 2.569345 with sigma of 0.02
3. Restrained planarity
 O1W, N3, N2, N1
 with sigma of 0.03
 O1W, H1WB, N3, N2, N1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C8(H8), C9(H9), C3(H3), C6(H6), C4(H4), C5(H5)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'