Two new <i>X</i>P(O)[NHC(CH~3~)~3~]~2~ phosphoramidates, with <i>X</i> = (CH~3~)~2~N and [(CH~3~)~3~CNH]~2~P(O)(O)
Pourayoubi, Mehrdad; Tarahhomi, Atekeh; Karimi Ahmadabad, Fatemeh; Fejfarová, Karla; van der Lee, Arie; Dušek, Michal; Acta Crystallographica Section C 68 (2012) o164–o169; doi:10.1107/S0108270112008566

data_2018451
_publ_section_title
;
 Two new <i>X</i>P(O)[NHC(CH~3~)~3~]~2~ phosphoramidates, with <i>X</i> =
 (CH~3~)~2~N and [(CH~3~)~3~CNH]~2~P(O)(O)
;
_journal_coeditor_code           FA3268
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o164
_journal_page_last               o169
_journal_paper_doi               10.1107/S0108270112008566
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C10 H26 N3 O P'
_chemical_formula_moiety         'C10 H26 N3 O P'
_chemical_formula_sum            'C10 H26 N3 O P'
_chemical_formula_weight         235.31
_chemical_name_common
;
<i>N</i>,<i>N</i>'-di-<i>tert</i>-butyl-<i>N</i>'',<i>N</i>''-
dimethylphosphoric triamide
;
_chemical_name_systematic
;
<i>tert</i>-butyl[(<i>tert</i>-butylamino)(dimethylamino)phosphoryl]amine
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90.529(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   12.0615(4)
_cell_length_b                   21.2567(7)
_cell_length_c                   17.1877(6)
_cell_measurement_reflns_used    11069
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.0679
_cell_measurement_theta_min      1.5206
_cell_volume                     4406.5(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2010)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2010)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2010)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material
;
CRYSTALS (Betteridge <i>et al.</i>, 2003) and enCIFer (Allen <i>et
al.</i>,
2004)
;
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Agilent Gemini-S with Sapphire3 detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_sigmaI/netI    0.1503
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29385
_diffrn_reflns_theta_full        26.217
_diffrn_reflns_theta_max         29.131
_diffrn_reflns_theta_min         1.524
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1560.006
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.57
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   0.00(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         17382
_refine_ls_number_restraints     207
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.0056128
_refine_ls_shift/su_mean         0.0001139
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method = Modified Sheldrick
w = 1/[\s^2^(F^2^) + ( 0.08P)^2^ + 1.62P], where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1609
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                11821
_reflns_number_total             17386
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3268.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2018451
_cod_database_fobs_code          2018451