An unprecedented cobalt(II)-containing Wells-Dawson-type tungstovanadate-based metal-organic framework as efficient catalyst for ring-opening polymerization of -caprolactone
Shen, Nan; Feng, Tian; Chang, Jun; Huang, Kunlin; Zhang, Zhi-Hui; Feng, Xuejun; Gu, Jiande; Chen, Sheng-Chun; He, Mingyang; Chen, Qun; CrystEngComm  (2020) –; doi:10.1039/D0CE00309C

data_7240382
_publ_section_title
;
 An unprecedented cobalt(II)-containing Wells-Dawson-type
 tungstovanadate-based metal-organic framework as efficient catalyst for
 ring-opening polymerization of &#xF065;-caprolactone
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00309C
_journal_year                    2020
_chemical_formula_moiety         'C60 H42 Co3 F20 N30 O64 V2 W18, 26(H2 O)'
_chemical_formula_sum            'C60 H96 Co3 F20 N30 O90 V2 W18'
_chemical_formula_weight         6645.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-22 deposited with the CCDC.	2020-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0649(6)
_cell_length_b                   30.3771(7)
_cell_length_c                   18.2553(5)
_cell_measurement_reflns_used    9504
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.43
_cell_volume                     13345.0(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            145996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.547
_diffrn_reflns_theta_min         2.300
_exptl_absorpt_coefficient_mu    16.082
_exptl_absorpt_correction_T_max  0.0709
_exptl_absorpt_correction_T_min  0.0601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.308
_exptl_crystal_description       block
_exptl_crystal_F_000             12100
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.35
_platon_squeeze_details
;
18 water molecules were removed from formula, the formula should be 
{[Co3(Fbtx)5(V2W18O62)(H2O)2] 18H2O}n before SQUEEZE.

TITL a_sq      P n n a      R = 0.07
CELL   24.0649   30.3771   18.2553     90.00     90.00     90.00
SPGR Pnna
C101 0.225 0.648 0.249 !       8.74 eA-3
C102 0.381 0.217 0.388 !       7.29 eA-3
C103 0.467 0.750 0.250 !       6.42 eA-3
Q104 0.165 0.767 0.029 !       6.02 eA-3
C105 0.062 0.830 0.204 !       5.93 eA-3
Q106 0.671 0.631 0.455 !       4.90 eA-3
Q107 0.656 0.221 0.392 !       4.88 eA-3
Q108 0.344 0.721 0.892 !       4.88 eA-3
Q109 0.789 0.386 0.246 !       4.86 eA-3
Q110 0.093 0.714 0.895 !       4.84 eA-3
C111 0.024 0.216 0.731 !       4.80 eA-3
C112 0.306 0.855 0.185 !       4.73 eA-3
C113 0.164 0.640 0.169 !       4.64 eA-3
Q114 0.625 0.224 0.390 !       4.59 eA-3
Q115 0.564 0.721 0.110 !       4.47 eA-3
Q116 0.211 0.274 0.467 !       4.31 eA-3
Q117 0.378 0.279 0.889 !       4.27 eA-3
Q118 0.586 0.673 0.295 !       4.23 eA-3
Q119 0.188 0.231 0.609 !       4.10 eA-3
Q120 0.553 0.674 0.293 !       3.94 eA-3
Q121 0.674 0.613 0.271 !       3.88 eA-3
C122 0.304 0.383 0.340 !       3.88 eA-3
C123 0.251 0.921 0.332 !       3.83 eA-3
Q124 0.827 0.331 0.061 !       3.79 eA-3
C125 0.351 0.708 0.238 !       3.76 eA-3
Q126 0.749 0.674 0.060 !       3.76 eA-3
Q127 0.212 0.677 0.920 !       3.75 eA-3
C128 0.250 1.001 0.438 !       3.74 eA-3
Q129 0.656 0.170 0.201 !       3.70 eA-3
Q130 0.807 0.829 0.202 !       3.65 eA-3
Q131 0.907 0.308 0.106 !       3.63 eA-3
Q132 0.833 0.182 0.001 !       3.61 eA-3
Q133 0.624 0.170 0.202 !       3.53 eA-3
Q134 0.378 0.329 0.709 !       3.38 eA-3
Q135 0.783 0.367 0.458 !       3.36 eA-3
C136 0.180 0.038 0.117 !       3.35 eA-3
Q137 0.208 0.374 0.541 !       3.34 eA-3
Q138 0.711 0.307 0.496 !       3.20 eA-3
Q139 0.155 0.255 0.621 !       3.18 eA-3
Q140 0.281 0.226 0.036 !       3.14 eA-3
Q141 0.902 0.177 0.017 !       3.04 eA-3
Q142 0.795 0.411 0.249 !       2.98 eA-3
Q143 0.243 0.265 0.476 !       2.94 eA-3
Q144 0.867 0.183 0.000 !       2.84 eA-3
C145 0.253 0.410 0.220 !       2.78 eA-3
Q146 0.914 0.362 0.293 !       2.71 eA-3
Q147 0.141 0.786 0.002 !       2.65 eA-3
Q148 0.838 0.638 0.317 !       2.58 eA-3
Q149 0.251 0.400 0.553 !       2.56 eA-3
C150 0.267 0.037 0.449 !       2.55 eA-3
Q151 0.711 0.641 0.065 !       2.53 eA-3
C152 0.381 0.250 0.250 !       2.44 eA-3
Q153 0.475 0.800 0.497 !       2.43 eA-3
C154 0.265 0.466 0.324 !       2.38 eA-3
Q155 0.227 0.165 0.031 !       2.38 eA-3
Q156 0.633 0.850 0.010 !       2.37 eA-3
Q157 0.586 0.700 0.305 !       2.31 eA-3
Q158 0.655 0.299 0.302 !       2.30 eA-3
C159 0.671 0.817 0.776 !       2.23 eA-3
Q160 0.069 0.295 0.017 !       2.22 eA-3
Q161 0.248 0.132 0.946 !       2.19 eA-3
Q162 0.795 0.295 0.084 !       2.18 eA-3
Q163 0.702 0.556 0.048 !       2.18 eA-3
Q164 0.311 0.376 0.501 !       2.12 eA-3
Q165 0.258 0.694 0.480 !       2.11 eA-3
Q166 0.178 0.208 0.279 !       2.09 eA-3
C167 0.226 0.964 0.121 !       2.03 eA-3
Q168 0.240 0.087 0.368 !       1.99 eA-3
Q169 0.767 1.004 0.252 !       1.95 eA-3
Q170 0.380 0.818-0.001 !       1.94 eA-3
Q171 0.709 0.723 0.340 !       1.91 eA-3
Q172 0.742 0.168 0.037 !       1.83 eA-3
Q173 0.734 0.152 0.072 !       1.81 eA-3
Q174 0.243 0.257 0.035 !       1.79 eA-3
C175 0.721 0.558 0.905 !       1.78 eA-3
C176 0.180 0.933 0.404 !       1.77 eA-3
C177 0.248 0.328 0.175 !       1.77 eA-3
C178 0.239 0.946 0.180 !       1.75 eA-3
C179 0.712 0.788 0.745 !       1.73 eA-3
Q180 0.227 0.703 0.457 !       1.73 eA-3
Q181 0.302 0.987 0.075 !       1.72 eA-3
C182 0.196 0.712 0.279 !       1.71 eA-3
Q183 0.071 0.070 0.126 !       1.70 eA-3
C184 0.618 0.832 0.779 !       1.70 eA-3
C185 0.672 0.757 0.766 !       1.68 eA-3
Q186 0.746 0.240 0.763 !       1.66 eA-3
C187 0.881 0.724 0.764 !       1.64 eA-3
Q188 0.710 0.271 0.747 !       1.62 eA-3
Q189 0.540 0.172 0.575 !       1.61 eA-3
C190 0.232 0.795 0.247 !       1.60 eA-3
Q191 0.157 0.384 0.873 !       1.60 eA-3
Q192 0.274 0.794 0.283 !       1.60 eA-3
Q193 0.593 0.979 0.115 !       1.59 eA-3
Q194 0.373 0.871 0.363 !       1.57 eA-3
Q195 0.741 0.876 0.111 !       1.52 eA-3
Q196 0.516 0.656 0.278 !       1.50 eA-3
Q197 0.109 0.390 0.484 !       1.50 eA-3
C198 0.805 0.243 0.774 !       1.48 eA-3
C199 0.747 0.888 0.764 !       1.47 eA-3
;
_refine_diff_density_max         5.771
_refine_diff_density_min         -1.710
_refine_diff_density_rms         0.415
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         13761
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+138.3690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.1784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10544
_reflns_number_total             13761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00309c2.cif
_cod_data_source_block           a_sq
_cod_database_code               7240382
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.071
_shelx_estimated_absorpt_t_min   0.060
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 O12, W7, O13, W9, O26, W8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C9(H9A,H9B), C16(H16A,H16B), C21(H21A,H21B), C28(H28A,H28B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C7(H7), C8(H8), C17(H17), C18(H18), C19(H19), C20(H20),
 C29(H29), C30(H30)
;
_shelx_res_checksum              88374
_shelx_fab_checksum              22637
_olex2_submission_special_instructions 'No special instructions were received'