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

data_4071672
_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            'C52 H62 Ca N2 O4 P2 Se2'
_chemical_formula_weight         1038.98
_chemical_name_common            '[(thf)2Ca{Pic(Se)PPh2}2]'
_chemical_name_systematic
; 
 Bis[diphenyl-(2-picolyl)phosphan selenide]calcium
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 96.9460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.690(2)
_cell_length_b                   9.1573(7)
_cell_length_c                   19.4842(14)
_cell_measurement_reflns_used    6050
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.595
_cell_measurement_theta_min      4.689
_cell_volume                     4904.3(6)
_computing_cell_refinement       'SAINT V7.23A'
_computing_data_collection       'APEX2 v2.1-4'
_computing_data_reduction        'SAINT V7.23A'
_computing_molecular_graphics    'XP in SHELXTL ver. 6.10'
_computing_publication_material  'XP in SHELXTL ver. 6.10'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25988
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.724
_exptl_absorpt_correction_T_max  0.8878
_exptl_absorpt_correction_T_min  0.7858
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2007/5
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         5030
_refine_ls_number_restraints     602
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0303P)^2^+6.4205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                4388
_reflns_number_total             5030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800307d_si_001.cif
_cod_data_source_block           3
_cod_original_cell_volume        4904.2(6)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4071672