Tetramethyl 1,1,2-triphenyl-2<i>H</i>-1λ^5^-phosphole-2,3,4,5-tetracarboxylate
Krawczyk, Krzysztof K.; Wojtasiewicz, Krystyna; Maurin, Jan K.; Gronowska, Ewa; Czarnocki, Zbigniew; Acta Crystallographica Section E 66 (2010) o2791–; doi:10.1107/S1600536810037827

data_2227344
_publ_section_title
;
 Tetramethyl
 1,1,2-triphenyl-2<i>H</i>-1\l^5^-phosphole-2,3,4,5-tetracarboxylate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2791
_journal_paper_doi               10.1107/S1600536810037827
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C30 H27 O8 P'
_chemical_formula_moiety         'C30 H27 O8 P'
_chemical_formula_sum            'C30 H27 O8 P'
_chemical_formula_weight         546.49
_chemical_melting_point          527
_chemical_name_systematic
;
Tetramethyl 1,1,2-triphenyl-2<i>H</i>-1\l^5^-phosphole-2,3,4,5-tetracarboxylate
;
_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                73.93(3)
_cell_angle_beta                 72.54(4)
_cell_angle_gamma                69.24(4)
_cell_formula_units_Z            2
_cell_length_a                   10.445(6)
_cell_length_b                   10.897(4)
_cell_length_c                   13.778(4)
_cell_measurement_reflns_used    13436
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.3114
_cell_measurement_theta_min      3.4118
_cell_volume                     1373.0(11)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'SHELXTL-NT (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4922
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur diffractometer with Ruby CCD
;
_diffrn_measurement_method       '\o and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20877
_diffrn_reflns_theta_full        70.87
_diffrn_reflns_theta_max         70.87
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    1.315
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.2024
_exptl_crystal_size_mid          0.1174
_exptl_crystal_size_min          0.0396
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+0.1050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1277
_reflns_number_gt                4503
_reflns_number_total             5207
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cv2752.cif
_cod_data_source_block           I
_cod_original_cell_volume        1373.0(10)
_cod_database_code               2227344
_cod_database_fobs_code          2227344