The molecular and crystal structures of the tris(dimethylamino)phosphoranes (Me2N)3P–X (X = BH3, CH2, NH or O)
Mitzel, Norbert W.; Lustig, Christian; Journal of the Chemical Society, Dalton Transactions  (1999) 3177–; doi:10.1039/a903292d

data_7027500
_publ_section_title
;
 The molecular and crystal structures of the
 tris(dimethylamino)phosphoranes (Me2N)3P--X (X&#x2005;=&#x2005;BH3, CH2,
 NH or O)
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3177
_journal_paper_doi               10.1039/a903292d
_journal_year                    1999
_chemical_compound_source        Fluka
_chemical_formula_sum            'C6 H19 N4 P'
_chemical_formula_weight         178.22
_chemical_melting_point          254.15
_chemical_name_systematic
; 
 Tris(dimethylamino)iminophosphorane 
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.512(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2190(9)
_cell_length_b                   10.0901(3)
_cell_length_c                   12.1644(14)
_cell_measurement_reflns_used    88
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     1000.14(16)
_computing_cell_refinement       'CAD4 Software'
_computing_data_collection       'CAD4 Software'
_computing_data_reduction        CADSHEL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(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  0.0134
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2863
_diffrn_reflns_theta_max         27.03
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        None
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       Column
_exptl_crystal_F_000             392
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.075
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2176
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_obs          0.0360
_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^)+(0.0714P)^2^+0.2105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1054
_refine_ls_wR_factor_obs         0.1006
_reflns_number_observed          1995
_reflns_number_total             2177
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903292Dsup1.cif
_cod_data_source_block           mit7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '-19' was changed to '254.15' - it
was converted from degrees Celsius(C) to
Kelvins(K).

'_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.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' 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^)+(0.0714P)^2^+0.2105P] 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^)+(0.0714P)^2^+0.2105P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1000.1(2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027500