A novel (4,8)-connected 3D polyoxometalate-based metal‒organic framework containing an in situ ligand
Lan, Ya-Qian; Li, Shun-Li; Li, Yang-Guang; Su, Zhong-Min; Shao, Kui-Zhan; Wang, Xin-Long; CrystEngComm 10 (2008) 1129–; doi:10.1039/b802627k

data_7202022
_publ_section_title
;
 A novel (4,8)-connected 3D polyoxometalate-based metal--organic
 framework containing an in situ ligand
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1129
_journal_paper_doi               10.1039/b802627k
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C28 H48 Cu4 N24 O50 P W12'
_chemical_formula_weight         4012.23
_chemical_name_systematic
;
?
;
_space_group_IT_number           71
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2'
_symmetry_space_group_name_H-M   'I m m m'
_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                   15.3782(19)
_cell_length_b                   16.460(2)
_cell_length_c                   20.120(3)
_cell_measurement_temperature    150(2)
_cell_volume                     5092.9(12)
_computing_cell_refinement       'SMART (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97(Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w 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  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15272
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.403
_exptl_absorpt_correction_T_max  0.1
_exptl_absorpt_correction_T_min  0.074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3606
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.646
_refine_diff_density_min         -3.367
_refine_diff_density_rms         0.347
_refine_ls_extinction_coef       0.00010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3394
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1072P)^2^+106.4521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.1821
_reflns_number_gt                2636
_reflns_number_total             3394
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802627k.txt
_cod_data_source_block           1
_cod_original_cell_volume        5093.1(11)
_cod_original_sg_symbol_H-M      Immm
_cod_database_code               7202022