Structural and Spectroscopic Studies of the PCP-Bridged Heavy Chalcogen-Centered Monoanions [HC(PPh2E)(PPh2)]- (E = Se, Te) and [HC(PR2E)2]- (E = Se, Te, R = Ph; E = Se, R =iPr): Homoleptic Group 12 Complexes and One-Electron Oxidation of [HC(PR2Se)2]-
Jari Konu; Heikki M. Tuononen; Tristram Chivers; Inorganic Chemistry 48 (2009) 11788–11798; doi:10.1021/ic901878h

data_4303903
_publ_section_title
;
Structural and Spectroscopic Studies of the PCP-Bridged Heavy
Chalcogen-Centered Monoanions [HC(PPh2E)(PPh2)]- (E = Se, Te) and
[HC(PR2E)2]- (E = Se, Te, R = Ph; E = Se, R =iPr): Homoleptic Group 12
Complexes and One-Electron Oxidation of [HC(PR2Se)2]-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11788
_journal_page_last               11798
_journal_paper_doi               10.1021/ic901878h
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C31 H37 Li N2 P2 Se2'
_chemical_formula_sum            'C31 H37 Li N2 P2 Se2'
_chemical_formula_weight         664.43
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.730(4)
_cell_length_b                   17.919(4)
_cell_length_c                   9.0249(18)
_cell_measurement_reflns_used    5409
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.27
_cell_volume                     3190.7(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'WinGX v1.70-01 (L. J. Farrugia)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'KappaCCD (Nonius, FR540C)'
_diffrn_measurement_method       'phi\omega scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'Enraf Nonius FR590D, fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5409
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.440
_exptl_absorpt_correction_T_max  0.8674
_exptl_absorpt_correction_T_min  0.7584
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (SHELXTL-NT v5.1, Bruker)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.521(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5409
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0140P)^2^+6.4324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                4239
_reflns_number_total             5409
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901878h_si_001_3.cif
_cod_data_source_block           compound_Li8a
_cod_original_cell_volume        3190.8(11)
_cod_database_code               4303903