Hydrothermal syntheses and structures of three one-dimensional heteropolytungstates formed by Dawson or Keggin cluster units
Yan, Bangbo; Xu, Yan; Bu, Xianhui; Goh, Ngoh K.; Chia, Lian S.; Stucky, Galen D.; Journal of the Chemical Society, Dalton Transactions  (2001) 2009–; doi:10.1039/b103024h

data_7010724
_publ_section_title
;
 Hydrothermal syntheses and structures of three one-dimensional
 heteropolytungstates formed by Dawson or Keggin cluster units
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2009
_journal_paper_doi               10.1039/b103024h
_journal_year                    2001
_chemical_formula_sum            'C15 H75 Cu4.5 N15 O68 P2 W17'
_chemical_formula_weight         5027.22
_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_date             'Sat FAB 10 08:57:58 2001'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.303(12)
_cell_angle_beta                 79.360(14)
_cell_angle_gamma                66.705(12)
_cell_formula_units_Z            2
_cell_length_a                   11.724(3)
_cell_length_b                   13.239(3)
_cell_length_c                   29.571(6)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      17.25
_cell_measurement_theta_min      2.62
_cell_volume                     4133.8(17)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0950
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            14257
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        13.65
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    24.821
_exptl_absorpt_correction_T_max  0.4368
_exptl_absorpt_correction_T_min  0.0502
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            PURPLE
_exptl_crystal_density_diffrn    4.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             4465
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.512
_refine_diff_density_min         -2.876
_refine_diff_density_rms         0.569
_refine_ls_extinction_coef       0.000152(17)
_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   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         12185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0732
_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^)+(0.0767P)^2^+159.4918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1709
_reflns_number_gt                8081
_reflns_number_total             12185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103024h.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4134.0(16)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C15 H75 Cu4.50 N15 O68 P2 W17'
_cod_database_code               7010724