Synthesis, properties and X-ray crystal structure of a new heteropolyacid supermolecular charge-transfer complex [(VB~1~)~2~DMFHPMo~12~O~40~·5DMF]
Liu, Shizhong; Li, Jianping; Feng, Xianhua; Cao, Zhengtai; Zhang, Zhenwen; Wang, Zheng; Xing, Yan; Jia, Hengqing; Lin, Yonghua; Acta Crystallographica Section B 58 (2002) 803–807; doi:10.1107/S010876810201008X

data_2103334
_publ_section_title
;
 Synthesis, properties and X-ray crystal structure of a new
 heteropolyacid supermolecular charge-transfer complex
 [(VB~1~)~2~DMFHPMo~12~O~40~&#x00B7;5DMF]
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              803
_journal_page_last               807
_journal_paper_doi               10.1107/S010876810201008X
_journal_volume                  58
_journal_year                    2002
_chemical_formula_sum            'C42 H76 Mo12 N14 O52 P S2'
_chemical_formula_weight         2855.54
_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
_cell_angle_alpha                103.900(3)
_cell_angle_beta                 98.87(3)
_cell_angle_gamma                112.85(3)
_cell_formula_units_Z            1
_cell_length_a                   12.322(3)
_cell_length_b                   13.607(3)
_cell_length_c                   14.160(3)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      9.73
_cell_measurement_theta_min      4.89
_cell_volume                     2040.9(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0792
_diffrn_reflns_av_sigmaI/netI    0.0790
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6706
_diffrn_reflns_theta_max         23.02
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    1.958
_exptl_absorpt_correction_T_max  0.99156
_exptl_absorpt_correction_T_min  0.50034
_exptl_crystal_density_diffrn    2.323
_exptl_crystal_F_000             1393
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.349
_refine_diff_density_min         -1.631
_refine_ls_extinction_coef       0.0159(11)
_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_all   1.118
_refine_ls_goodness_of_fit_obs   1.198
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         5407
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.328
_refine_ls_restrained_S_obs      1.198
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_obs          0.0893
_refine_ls_shift/esd_max         3.172
_refine_ls_shift/esd_mean        0.361
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+51.6101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2676
_refine_ls_wR_factor_obs         0.2188
_reflns_number_observed          4509
_reflns_number_total             5563
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            an0598.cif
_cod_data_source_block           I
_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 

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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+51.6101P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+51.6101P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2040.9(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2103334