Organic‒inorganic hybrids based on four-electron reduced Keggin β-isomer phosphododecamolybdates and diazines
Vitoria, Pablo; Ugalde, María; Gutiérrez-Zorrilla, Juan M.; Román, Pascual; Luque, Antonio; San Felices, Leire; García-Tojal, Javier; New Journal of Chemistry 27 (2003) 399–; doi:10.1039/b207243b

data_7050434
_publ_section_title
;
 Organic--inorganic hybrids based on four-electron reduced Keggin
 \b-isomer phosphododecamolybdates and diazines
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              399
_journal_paper_doi               10.1039/b207243b
_journal_volume                  27
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'H4 Mo12 O40 P, 3(C4 H5 N2), 9(H2 O)'
_chemical_formula_sum            'C12 H37 Mo12 N6 O49 P'
_chemical_formula_weight         2231.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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             2002-07-22T18:11:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                72.04(9)
_cell_angle_beta                 79.76(12)
_cell_angle_gamma                62.95(9)
_cell_formula_units_Z            2
_cell_length_a                   12.6880(18)
_cell_length_b                   12.853(11)
_cell_length_c                   18.60(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.2
_cell_measurement_theta_min      11.3
_cell_measurement_wavelength     0.71069
_cell_volume                     2567(5)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF99.2
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.020762
_diffrn_orient_matrix_UB_12      0.087278
_diffrn_orient_matrix_UB_13      -0.006594
_diffrn_orient_matrix_UB_21      -0.029733
_diffrn_orient_matrix_UB_22      0.020395
_diffrn_orient_matrix_UB_23      -0.051267
_diffrn_orient_matrix_UB_31      -0.080873
_diffrn_orient_matrix_UB_32      0.012328
_diffrn_orient_matrix_UB_33      0.023231
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.017
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15291
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         1.8
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.983
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
DIFABS (Walker, N.; Stuart, D. Acta Cryst. 1983, A39, 158.)
;
_exptl_crystal_colour            'Dark blue'
_exptl_crystal_density_diffrn    2.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2124
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.205
_refine_diff_density_min         -3.001
_refine_diff_density_rms         0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         14863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0706P)^2^+11.1013P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.132
_refine_ls_wR_factor_ref         0.1343
_reflns_number_gt                13239
_reflns_number_total             14863
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207243b.txt
_cod_data_source_block           1
_cod_original_cell_volume        2567(4)
_cod_original_formula_sum        'C12 H37 Mo12 N6 O49 P1'
_cod_database_code               7050434
_diffrn_standards_decay_corr_max 1.148
_diffrn_standards_decay_corr_min 0.958