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_7050436
_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         'C10 H27 Mo12 N5 O45 P1'
_chemical_formula_sum            'C10 H27 Mo12 N5 O45 P'
_chemical_formula_weight         2119.62
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2002-07-22T18:11:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1820(10)
_cell_length_b                   21.356(3)
_cell_length_c                   21.703(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.7
_cell_measurement_theta_min      11.3
_cell_measurement_wavelength     0.71073
_cell_volume                     4639.5(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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      0.098392
_diffrn_orient_matrix_UB_12      -0.003685
_diffrn_orient_matrix_UB_13      0.001433
_diffrn_orient_matrix_UB_21      -0.014727
_diffrn_orient_matrix_UB_22      0.003274
_diffrn_orient_matrix_UB_23      -0.046714
_diffrn_orient_matrix_UB_31      0.008934
_diffrn_orient_matrix_UB_32      0.046727
_diffrn_orient_matrix_UB_33      0.003433
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13775
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         1.35
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        34
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.285
_exptl_absorpt_correction_T_max  0.3447
_exptl_absorpt_correction_T_min  0.5446=09
_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    3.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4004
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.961
_refine_diff_density_min         -2.616
_refine_diff_density_rms         0.303
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         13454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0781P)^2^+26.5764P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                10780
_reflns_number_total             13454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207243b.txt
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7050436
_diffrn_standards_decay_corr_max 1.574
_diffrn_standards_decay_corr_min 0.906