Low Symmetry in P(NR2)3 Skeletons and Related Fragments: An Inherent Phenomenon
Norbert W. Mitzel; Bruce A. Smart; Karl-Heinz Dreihäupl; David W. H. Rankin; Hubert Schmidbaur; Journal of the American Chemical Society 118 (1996) 12673–12682; doi:10.1021/ja9621861

data_4117219
_publ_section_title
;
 Low Symmetry in P(NR2)3 Skeletons and Related Fragments: An Inherent
 Phenomenon
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12673
_journal_page_last               12682
_journal_paper_doi               10.1021/ja9621861
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C7 H20 N3 P'
_chemical_formula_weight         177.23
_chemical_name_systematic
; 
 Tris(dimethylamino)methylene-phosphorane 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.593(2)
_cell_length_b                   12.446(3)
_cell_length_c                   7.297(3)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      12
_cell_volume                     1052.9(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            1496
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         3.24
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       Cylinder
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.35(24)
_refine_ls_extinction_coef       0.0023(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.019
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1336
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_obs          0.0479
_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^)+(0.0508P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1112
_refine_ls_wR_factor_obs         0.0960
_reflns_number_observed          936
_reflns_number_total             1338
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9621861_2.cif
_cod_data_source_block           npylid
_cod_depositor_comments
;Adding Fobs data.

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.0000P] 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^)+(0.0508P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4117219
_cod_database_fobs_code          4117219