A new 3D POMOF with two channels consisting of Wells‒Dawson arsenotungstate and {Cl4Cu10(pz)11} complexes: synthesis, crystal structure, and properties
Cong, Bo-Wen; Su, Zhan-Hua; Zhao, Zhi-Feng; Zhao, Wen-Qi; Ma, Xiu-Juan; Xu, Qiu; Du, Li-Juan; New Journal of Chemistry 42 (2018) 4596–; doi:10.1039/C7NJ04854H

data_7057034
_publ_section_title
;
 A new 3D POMOF with two channels consisting of Wells--Dawson
 arsenotungstate and {Cl4Cu10(pz)11} complexes: synthesis, crystal
 structure, and properties
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4596
_journal_paper_doi               10.1039/C7NJ04854H
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C22 H22 As Cl2 Cu5 N11 O31 W9, 0.75(H2 O)'
_chemical_formula_sum            'C22 H23.5 As Cl2 Cu5 N11 O31.75 W9'
_chemical_formula_weight         3068.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-07-31
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.06.29 svn.r3433 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2017-12-02 deposited with the CCDC.
2018-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.0750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.5445(19)
_cell_length_b                   14.3006(10)
_cell_length_c                   27.9545(19)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.43
_cell_volume                     10342.4(12)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0561
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            36483
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.428
_exptl_absorpt_coefficient_mu    22.772
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1728 before and 0.0663 after correction.
The Ratio of minimum to maximum transmission is 0.3648.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    3.941
_exptl_crystal_description       block
_exptl_crystal_F_000             10912
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.897
_refine_diff_density_min         -2.623
_refine_diff_density_rms         0.434
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         9614
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0776P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7788
_reflns_number_total             9614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj04854h2.cif
_cod_data_source_block           aa1_0m
_cod_depositor_comments          'Adding full bibliography for 7057034.cif.'
_cod_original_cell_volume        10342.3(12)
_cod_original_formula_sum        'C22 H23.50 As Cl2 Cu5 N11 O31.75 W9'
_cod_database_code               7057034
_shelx_shelxl_version_number     2016/6
_exptl_absorpt_special_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) = Uanis(O13)
Uanis(O1) = Uanis(O17)
Uanis(O9) = Uanis(O2)
Uanis(O14) = Uanis(O24)
3. Others
 Fixed Sof: O32(0.75) H32A(0.75) H32B(0.75)
4.a Riding coordinates:
 O32(H32A,H32B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C8(H8), C1(H1), C7(H7), C4(H4), C9(H9), C17(H17), C2(H2),
 C6(H6), C15(H15), C22(H22), C21(H21), C16(H16), C11(H11), C10(H10), C12(H12),
 C13(H13), C14(H14), C19(H19), C20(H20), C18(H18)
;
_shelx_res_checksum              95816
_olex2_submission_special_instructions 'No special instructions were received'