A monomeric <i>N</i>,<i>N</i>'-dilithiobis(amido)organophosphane
Copsey, May C.; Chivers, Tristram; Acta Crystallographica Section E 62 (2006) m1560–m1561; doi:10.1107/S1600536806021945

data_2209603
_publ_section_title
;
 A monomeric <i>N</i>,<i>N</i>'-dilithiobis(amido)organophosphane
;
_journal_coeditor_code           LH2099
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1560
_journal_page_last               m1561
_journal_paper_doi               10.1107/S1600536806021945
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Li2 (C30 H39 N2 P) (C4 H10 O)2]'
_chemical_formula_moiety         'C38 H59 Li2 N2 O2 P'
_chemical_formula_sum            'C38 H59 Li2 N2 O2 P'
_chemical_formula_weight         620.72
_chemical_name_systematic
;
[\m~2~-bis(2,6-diisopropylphenylamido)phenylphosphine]bis(diethyl
ether)dilithium(I)
;
_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                 109.78(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.679(3)
_cell_length_b                   15.381(3)
_cell_length_c                   16.734(3)
_cell_measurement_reflns_used    12831
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.99
_cell_volume                     3797.4(14)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12831
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_correction_T_min  0.9693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+1.8002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                4532
_reflns_number_total             6675
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2099.cif
_cod_data_source_block           I
_cod_original_cell_volume        3797.7(13)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2209603
_cod_database_fobs_code          2209603