Tris(triphenylsilyl)phosphate dichloromethane solvate
Ferguson, George; O'Leary, Brian J.; Spalding, Trevor R.; Acta Crystallographica Section E 61 (2005) o906–o907; doi:10.1107/S1600536805006604

data_2205545
_publ_section_title
;
 Tris(triphenylsilyl)phosphate dichloromethane solvate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o906
_journal_page_last               o907
_journal_paper_doi               10.1107/S1600536805006604
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C54 H45 O4 P Si3, 0.263C H2 Cl2'
_chemical_formula_moiety         'C54 H45 O4 P Si3, 0.263C H2 Cl2'
_chemical_formula_sum            'C54.26 H45.53 Cl0.53 O4 P Si3'
_chemical_formula_weight         895.48
_chemical_name_systematic
;
Tris(triphenylsilyl)phosphate dichloromethane solvate
;
_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
_cell_angle_alpha                91.75(2)
_cell_angle_beta                 105.47(2)
_cell_angle_gamma                106.31(2)
_cell_formula_units_Z            2
_cell_length_a                   10.284(2)
_cell_length_b                   13.055(3)
_cell_length_c                   19.015(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.0(10)
_cell_measurement_theta_max      14.00
_cell_measurement_theta_min      6.15
_cell_volume                     2346.0(9)
_computing_cell_refinement       DIFRAC
_computing_data_collection
'DIFRAC with profile analysis (Gabe & White, 1993)'
_computing_data_reduction        'DATRD2 in NRCVAX94 (Gabe et al., 1989)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement
'SHELXL97 (Sheldrick, 1997) in WinGX (Version 1.70.01; Farrugia, 1999)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      294.0(10)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.1786
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10183
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.93
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        3.8
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             938.1
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         10183
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.1763
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0501P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                4004
_reflns_number_total             10183
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6381.cif
_cod_data_source_block           I
_cod_database_code               2205545
_cod_database_fobs_code          2205545