A noncovalently connected metal‒organic framework assembled from a Ni(iii)-supported polyoxometalate‒imidazolate hybrid
Jiao, Yan-Qing; Li, Meng-Ting; Qin, Chao; Su, Zhong-Min; CrystEngComm 19 (2017) 1721–; doi:10.1039/C6CE02420C

data_7227487
_publ_section_title
;
 A noncovalently connected metal--organic framework assembled from a
 Ni(iii)-supported polyoxometalate--imidazolate hybrid
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1721
_journal_paper_doi               10.1039/C6CE02420C
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety
'C4 H6 N2 Ni O39 Si W11, C16 H24 N8 Ni, C4 H7 N2, O'
_chemical_formula_sum            'C24 H45 N12 Ni2 O42 Si W11'
_chemical_formula_weight         3341.38
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-01-16 deposited with the CCDC.
2017-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   49.6795(9)
_cell_length_b                   49.6795(9)
_cell_length_c                   23.7404(8)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.695
_cell_measurement_theta_min      2.420
_cell_volume                     50743(2)
_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      173.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            126387
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.733
_diffrn_reflns_theta_min         2.235
_exptl_absorpt_coefficient_mu    11.562
_exptl_absorpt_correction_T_max  0.125
_exptl_absorpt_correction_T_min  0.095
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_description       block
_exptl_crystal_F_000             26730
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.033
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         21441
_refine_ls_number_restraints     786
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0529P)^2^+389.4638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16420
_reflns_number_total             21441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce02420c2.cif
_cod_data_source_block           1028317
_cod_depositor_comments          'Adding full bibliography for 7227487.cif.'
_cod_original_cell_volume        50743(3)
_cod_database_code               7227487
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim N1
\\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8 \\sim N9 \\sim
N10 \\sim N11 \\sim N12: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.03
Uiso(O1WA) = Uiso(O1WB)
3. Others
 Sof(O1WB)=1-FVAR(1)
 Sof(O1WA)=FVAR(1)
4.a Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C),
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2A), C3(H3), N3(H3A), N5(H5), N7(H7), N9(H9), C5(H5A), C6(H6),
 C9(H9A), C10(H10), C13(H13), C14(H14), C17(H17), C18(H18), N11(H11), N12(H12),
 C21(H21), C22(H22)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              5568
_olex2_submission_special_instructions 'No special instructions were received'