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_4117218
_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            'C6 H18 N3 P'
_chemical_formula_weight         163.20
_chemical_name_systematic
; 
 Tris(dimethylamino)phosphane 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                80.45(3)
_cell_angle_beta                 80.54(3)
_cell_angle_gamma                80.86(3)
_cell_formula_units_Z            4
_cell_length_a                   6.184(2)
_cell_length_b                   11.471(4)
_cell_length_c                   14.676(5)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      15.0
_cell_volume                     1003.4(6)
_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  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4130
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.84
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       Cylinder
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.0034(47)
_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   1.016
_refine_ls_goodness_of_fit_obs   1.055
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.192
_refine_ls_restrained_S_obs      1.055
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_obs          0.0631
_refine_ls_shift/esd_max         -0.038
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1412P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2266
_refine_ls_wR_factor_obs         0.1699
_reflns_number_observed          2607
_reflns_number_total             3545
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9621861_1.cif
_cod_data_source_block           pnme23
_cod_depositor_comments
;Adding Fobs data.

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1412P)^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^)+(0.1412P)^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               4117218
_cod_database_fobs_code          4117218