Combined XRD and infrared studies of pyridinium species in (PyH)(3)[PW(12)O(40)] single crystals.
Pichon, Céline; Mialane, Pierre; Marrot, Jérôme; Binet, Claude; Vimont, Alexandre; Travert, Arnaud; Lavalley, Jean-Claude; Physical chemistry chemical physics : PCCP 13 (2011) 322–327; doi:10.1039/c0cp00446d

data_7205528
_publ_section_title
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 Combined XRD and infrared studies of pyridinium species in
 (PyH)(3)[PW(12)O(40)] single crystals.
;
_journal_issue                   1
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              322
_journal_page_last               327
_journal_paper_doi               10.1039/c0cp00446d
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C19 H24 N5 O40 P W12'
_chemical_formula_weight         3199.60
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 119.933(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.5058(4)
_cell_length_b                   14.3158(4)
_cell_length_c                   16.6984(5)
_cell_measurement_reflns_used    8788
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.13
_cell_measurement_theta_min      2.53
_cell_volume                     4869.6(2)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            128879
_diffrn_reflns_theta_full        30.15
_diffrn_reflns_theta_max         30.15
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    28.359
_exptl_absorpt_correction_T_max  0.3967
_exptl_absorpt_correction_T_min  0.0701
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    4.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5584
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.839
_refine_diff_density_min         -4.651
_refine_diff_density_rms         0.937
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         7200
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+162.9977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                6592
_reflns_number_total             7200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CP00446D.TXT
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'multi-scans' was replaced
with 'multi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4869.5(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7205528