Multidimensional crystal frameworks based on heteropoly blue building block of [SiW10Mo(V)2O40]6-: synthesis, structures and magnetic properties.
Wang, Yuchao; Li, Fengyan; Xu, Lin; Jiang, Ning; Liu, Xizheng; Dalton transactions (Cambridge, England : 2003) 42 (2013) 5839–5847; doi:10.1039/c3dt32658f

data_7022650
_publ_section_title
;
 Multidimensional crystal frameworks based on heteropoly blue building
 block of [SiW10Mo(V)2O40]6-: synthesis, structures and magnetic
 properties.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5839
_journal_page_last               5847
_journal_paper_doi               10.1039/c3dt32658f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C36 H84 Cu K4.88 Mo4 N12 Na1.13 O92 Si2 W20'
_chemical_formula_weight         6554.11
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.78
_cell_angle_beta                 75.26
_cell_angle_gamma                61.18
_cell_formula_units_Z            1
_cell_length_a                   12.535
_cell_length_b                   12.729
_cell_length_c                   21.473
_cell_measurement_reflns_used    7277
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1585
_cell_measurement_theta_min      2.9474
_cell_volume                     2892.549
_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, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Smart CCD Apex II'
_diffrn_measurement_method       'omega and phi'
_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  0.0419
_diffrn_reflns_av_unetI/netI     0.1095
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17251
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    21.024
_exptl_absorpt_correction_T_max  0.023
_exptl_absorpt_correction_T_min  0.005
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            darkslategray
_exptl_crystal_density_diffrn    3.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2948.6
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.198
_refine_diff_density_min         -4.040
_refine_diff_density_rms         0.492
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         10138
_refine_ls_number_restraints     1552
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                6451
_reflns_number_total             10138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32658f.txt
_cod_data_source_block           3D
_cod_original_cell_volume        2892.6
_cod_original_sg_symbol_H-M      'p -1'
_cod_database_code               7022650