Lithiated organophosphorus enamines: a new synthetic approach and the first crystal structures
Clegg, William; Liddle, Stephen T.; Davies, Robert P.; Dunbar, Lorraine; Feeder, Neil; Snaith, Ronald; Wheatley, Andrew E. H.; Mulvey, Robert E.; Chemical Communications  (1999) 1401–; doi:10.1039/a903175h

data_7110569
_publ_section_title
;
 Lithiated organophosphorus enamines: a new synthetic approach and the
 first crystal structures
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1401
_journal_paper_doi               10.1039/a903175h
_journal_year                    1999
_chemical_formula_sum            'C21 H29 Li N2 O P'
_chemical_formula_weight         363.37
_chemical_name_systematic
; 
 ? 
;
_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                 130.69(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.740(6)
_cell_length_b                   9.803(2)
_cell_length_c                   20.206(4)
_cell_measurement_temperature    180(2)
_cell_volume                     4166(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1087
_diffrn_reflns_av_sigmaI/netI    0.1364
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7372
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.9720
_exptl_absorpt_correction_T_min  0.9652
_exptl_absorpt_correction_type   Psi-Scans
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                1998
_reflns_number_total             3669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903175hsup1.cif
_cod_data_source_block           rs9818
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4166.6(14)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7110569