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_7027499
_publ_section_title
;
 The molecular and crystal structures of the
 tris(dimethylamino)phosphoranes (Me2N)3P--X (X&#x2005;=&#x2005;BH3, CH2,
 NH or O)
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_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_formula_sum            'C6 H21 B N3 P'
_chemical_formula_weight         177.04
_chemical_melting_point          292
_chemical_name_systematic
; 
 tris(dimethylamino)phosphane-borane 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 96.29(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.996(2)
_cell_length_b                   11.174(1)
_cell_length_c                   7.679(1)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      22
_cell_volume                     1108.4(2)
_computing_cell_refinement       CAD4-Software
_computing_data_collection       CAD4-Software
_computing_data_reduction        CADSHEL
_computing_molecular_graphics    SHELXTL-5.01
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      158(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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4672
_diffrn_reflns_theta_max         27.05
_diffrn_reflns_theta_min         3.15
_diffrn_standards_decay_%        None
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       Block
_exptl_crystal_F_000             392
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(6)
_refine_ls_extinction_coef       0.0015(9)
_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   1.083
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2398
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.097
_refine_ls_restrained_S_obs      1.087
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_obs          0.0207
_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^)+(0.0361P)^2^+0.0772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0556
_refine_ls_wR_factor_obs         0.0543
_reflns_number_observed          2335
_reflns_number_total             2399
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903292Dsup1.cif
_cod_data_source_block           lus2
_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^)+(0.0361P)^2^+0.0772P] 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^)+(0.0361P)^2^+0.0772P] 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      Cc
_cod_database_code               7027499