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_2018452
_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          'C16 H40 N4 O3 P2'
_chemical_formula_moiety         'C16 H40 N4 O3 P2'
_chemical_formula_sum            'C16 H40 N4 O3 P2'
_chemical_formula_weight         398.5
_chemical_name_common
;
<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>'''-tetra-<i>tert</i>-
butyloxybis(phosphonic diamide)
;
_chemical_name_systematic
;
({[bis(tert-butylamino)phosphoryl]oxy}(<i>tert</i>-
butylamino)phosphoryl)(<i>tert</i>-butyl)amine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 119.371(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3715(4)
_cell_length_b                   17.7755(7)
_cell_length_c                   13.6956(5)
_cell_measurement_reflns_used    9398
_cell_measurement_temperature    150
_cell_measurement_theta_max      67.05
_cell_measurement_theta_min      3.7
_cell_volume                     2412.51(18)
_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
;
JANA2006 (Pet\<r\'i\<cek <i>et al.</i>, 2006) and enCIFer (Allen <i>et
al.</i>, 2004)
;
_computing_structure_refinement  'JANA2006 (Pet\<r\'i\<cek <i>et al.</i>, 2006)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type
'Gemini Ultra diffractometer with Atlas detector'
_diffrn_measurement_method
'Rotation method data acquisition using \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15622
_diffrn_reflns_reduction_process
;
Integration of the CCD images was done by program <i>CrysAlis PRO</i>
(Agilent, 2010). The same program was used for indexing of the
crystal shape and absorption correction.
;
_diffrn_reflns_theta_full        67.15
_diffrn_reflns_theta_max         67.15
_diffrn_reflns_theta_min         4.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.795
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.0967
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.60
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    148
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4265
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.0015
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/(\s^2^(I)+0.0016I^2^)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                3420
_reflns_number_total             4265
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            fa3268.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018452
_cod_database_fobs_code          2018452