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_7110568
_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            'C18.88 H22.25 Li N O P'
_chemical_formula_weight         317.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.472(2)
_cell_length_b                   16.472(2)
_cell_length_c                   13.664(3)
_cell_measurement_temperature    180(2)
_cell_volume                     3707.4(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6540
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.80
_exptl_absorpt_coefficient_mu    0.150
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.068
_refine_ls_goodness_of_fit_obs   1.112
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_restrained_S_obs      1.112
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_obs          0.0618
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+3.7737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2018
_refine_ls_wR_factor_obs         0.1774
_reflns_number_observed          2390
_reflns_number_total             3270
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903175hsup1.cif
_cod_data_source_block           rs9820
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+3.7737P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+3.7737P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P4/n
_cod_database_code               7110568