Synthesis of silicophosphates containing SiO~6~-octahedra under ambient conditions - reactions of anhydrous H~3~PO~4~ with alkoxysilanes
Sandra Jahnigen; Erica Brendler; Uwe Bohme; Edwin Kroke; Chem.Commun. 48 (2012) 7675–; doi:10.1039/c2cc31600e

data_7108070
_publ_section_title
;
 Synthesis of silicophosphates containing SiO~6~-octahedra under ambient
 conditions - reactions of anhydrous H~3~PO~4~ with alkoxysilanes
;
_journal_name_full               Chem.Commun.
_journal_page_first              7675
_journal_paper_doi               10.1039/c2cc31600e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C24 H60 O36 P6 Si7, 4(C H Cl3), 2(C6 H16 N)'
_chemical_formula_sum            'C40 H96 Cl12 N2 O36 P6 Si7'
_chemical_formula_weight         1989.04
_chemical_melting_point          536
_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-97
_cell_angle_alpha                94.538(2)
_cell_angle_beta                 98.483(2)
_cell_angle_gamma                95.689(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4825(3)
_cell_length_b                   15.5104(4)
_cell_length_c                   25.7924(8)
_cell_measurement_reflns_used    67066
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      1.48
_cell_volume                     4500.4(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      ' 364 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0978
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            71593
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.80
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  0.9554
_exptl_absorpt_correction_T_min  0.7939
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-RED; Stoe, 2009'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1030
_refine_ls_number_reflns         20118
_refine_ls_number_restraints     851
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1285P)^2^+4.6875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2207
_refine_ls_wR_factor_ref         0.2453
_reflns_number_gt                12527
_reflns_number_total             20118
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc31600e.txt
_cod_data_source_block           sj119_6
_cod_database_code               7108070