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_7027501
_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        'Aldrich Chemicals'
_chemical_formula_sum            'C6 H18 N3 O P'
_chemical_formula_weight         179.20
_chemical_melting_point          7
_chemical_name_common            HMPA
_chemical_name_systematic
; 
Tris(dimethylamino)oxophosphorane 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 104.19(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.398(1)
_cell_length_b                   12.570(3)
_cell_length_c                   6.428(1)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      20
_cell_volume                     501.18(18)
_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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3326
_diffrn_reflns_theta_max         31.09
_diffrn_reflns_theta_min         3.24
_diffrn_standards_decay_%        None
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       Column
_exptl_crystal_F_000             196
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.075
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_restrained_S_obs      1.075
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_obs          0.0427
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0809P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1162
_refine_ls_wR_factor_obs         0.1063
_reflns_number_observed          1345
_reflns_number_total             1671
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903292Dsup1.cif
_cod_data_source_block           mit6
_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.

'_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^)+(0.0809P)^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^)+(0.0809P)^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_original_cell_volume        501.2(2)
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               7027501