Synthesis and Characterization of a Stable Cyclicgem-Bis(phosphaylide): a 4π-Electron Three-Membered Heterocycle
Nicola Dellus; Tsuyoshi Kato; Nathalie Saffon-Merceron; Vicenç Branchadell; Antoine Baceiredo; Inorganic Chemistry 50 (2011) 7949–7951; doi:10.1021/ic2013182

data_4326203
_publ_section_title
;
 Synthesis and Characterization of a Stable Cyclicgem-Bis(phosphaylide): a
 4\p-Electron Three-Membered Heterocycle
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7949
_journal_page_last               7951
_journal_paper_doi               10.1021/ic2013182
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C42 H75 F N6 O0.5 P3 Si'
_chemical_formula_weight         812.08
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.7150(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6883(5)
_cell_length_b                   12.2323(3)
_cell_length_c                   20.8155(5)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.51
_cell_measurement_theta_min      2.18
_cell_volume                     4742.3(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            70434
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         5.12
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  0.9812
_exptl_absorpt_correction_T_min  0.9026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       plate
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         11515
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0671P)^2^+1.4911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                8043
_reflns_number_total             11515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2013182_si_001_2.cif
_cod_data_source_block           11
_cod_original_formula_sum        'C42 H75 F N6 O0.50 P3 Si'
_cod_database_code               4326203