Controlled synthesis of a functionalized polytungstate ligand and a {MaMbMc(PW9)2} sandwich complex
Cao, Rui; O'Halloran, Kevin P.; Hillesheim, Daniel A.; Lense, Sheri; Hardcastle, Kenneth I.; Hill, Craig L.; CrystEngComm 13 (2011) 738–; doi:10.1039/c0ce00828a

data_7205535
_publ_section_title
;
 Controlled synthesis of a functionalized polytungstate ligand and a
 {MaMbMc(PW9)2} sandwich complex
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              738
_journal_paper_doi               10.1039/c0ce00828a
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C6 H5 K9.75 O87.50 P2 Sn W19'
_chemical_formula_sum            'C6 H5 K9.75 O87.5 P2 Sn W19'
_chemical_formula_weight         5532.10
_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                109.785(8)
_cell_angle_beta                 95.200(8)
_cell_angle_gamma                94.589(9)
_cell_formula_units_Z            4
_cell_length_a                   11.809(7)
_cell_length_b                   24.155(13)
_cell_length_c                   35.310(19)
_cell_measurement_reflns_used    9447
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.15
_cell_measurement_theta_min      2.26
_cell_volume                     9372(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0668
_diffrn_reflns_av_sigmaI/netI    0.0671
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            170688
_diffrn_reflns_theta_full        30.37
_diffrn_reflns_theta_max         30.37
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    24.048
_exptl_absorpt_correction_T_max  0.2208
_exptl_absorpt_correction_T_min  0.0434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.920
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9649
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         6.183
_refine_diff_density_min         -3.333
_refine_diff_density_rms         0.517
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1345
_refine_ls_number_reflns         52507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+422.1635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                42769
_reflns_number_total             52507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00828A.TXT
_cod_data_source_block           2a
_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 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_cell_volume        9373(9)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C6 H5 K9.75 O87.50 P2 Sn W19'
_cod_database_code               7205535