A Dihydrate Complex of Molybdosilicic Acid and Hexamethylphosphoramide, [{(CH~3~)~2~N}~3~PO]~5~[H~4~SiMo~12~O~40~].2H~2~O
Fun, Hoong-Kun; Chinnakali, Kandasamy; Yip, Boon-Chuan; Niu, Jing-Yang; Wang, Jing-Ping; You, Xiao-Zeng; Acta Crystallographica Section C 54 (1998) 327–329; doi:10.1107/S0108270197015850

data_2007109
_publ_section_title
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 A Dihydrate Complex of Molybdosilicic Acid and
 Hexamethylphosphoramide,
 [{(CH~3~)~2~N}~3~PO]~5~[H~4~SiMo~12~O~40~].2H~2~O
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              327
_journal_page_last               329
_journal_paper_doi               10.1107/S0108270197015850
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '(C6 H18 N3 O P)5 [H4 Si Mo12 O40], 2H2 O'
_chemical_formula_moiety         'C30 H94 Mo12 N15 O47 P5 Si'
_chemical_formula_sum            'C30 H94 Mo12 N15 O47 P5 Si'
_chemical_formula_weight         2755.41
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                95.770(10)
_cell_angle_beta                 99.450(10)
_cell_angle_gamma                91.510(10)
_cell_formula_units_Z            2
_cell_length_a                   13.8490(10)
_cell_length_b                   13.9400(10)
_cell_length_c                   22.024(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5
_cell_volume                     4168.9(6)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL/PC
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \q/2\q
_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  0.021
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21390
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        <3
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.947
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_type   'empirical \y scans (XSCANS; Siemens, 1994)'
_exptl_crystal_colour
'Yellow in the dark and turning green when exposed to sunlight'
_exptl_crystal_density_diffrn    2.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.38
_refine_diff_density_min         -1.36
_refine_ls_extinction_coef       0.00099(7)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   0.961
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1084
_refine_ls_number_reflns         19037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.065
_refine_ls_R_factor_obs          .044
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0757P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.125
_refine_ls_wR_factor_obs         .116
_reflns_number_observed          13504
_reflns_number_total             19037
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            mu1354.cif
_cod_data_source_block           aniu15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0757P)^2^] 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^)+(0.0757P)^2^]
where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               2007109