Heteroaromatic Substituted Phosphoranes with Enhanced Hemilabile Character
Kling, Christian; Ott, Holger; Schwab, Gerald; Stalke, Dietmar; Organometallics 27 (2008) 5038–; doi:10.1021/om800307d

data_4071671
_publ_contact_author             'Prof. Dr. Dietmar Stalke'
_publ_section_title
;
 Heteroaromatic Substituted Phosphoranes with Enhanced Hemilabile
 Character
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5038
_journal_paper_doi               10.1021/om800307d
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C18 H16 N P Se'
_chemical_formula_weight         356.25
_chemical_name_common            Se=P(Pic)Ph2
_chemical_name_systematic        'Diphenyl-(2-picolyl)phosphane selenide'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.1020(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6149(7)
_cell_length_b                   7.2983(4)
_cell_length_c                   17.4007(10)
_cell_measurement_reflns_used    21604
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.19
_cell_volume                     1577.20(15)
_computing_cell_refinement       'SAINT V7.23A'
_computing_data_collection       'APEX2 v2.0-2'
_computing_data_reduction        'SAINT V7.23A'
_computing_molecular_graphics    'XP in SHELXTL ver. 6.12'
_computing_publication_material  'XP in SHELXTL ver. 6.12'
_computing_structure_refinement  'SHELXL in SHELXTL ver. 6.12'
_computing_structure_solution    'SHELXS in SHELXTL ver. 6.12'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       '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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0108
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37857
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    2.474
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2004/1
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0179
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.6560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0502
_reflns_number_gt                3078
_reflns_number_total             3220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800307d_si_001.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4071671