Syntheses and structures of four new mixed-amide phosphoric triamides.
Keikha, Mojtaba; Pourayoubi, Mehrdad; Tarahhomi, Atekeh; van der Lee, Arie; Acta crystallographica. Section C, Structural chemistry 72 (2016) 251–259; doi:10.1107/S2053229616001595

data_2311850
_publ_section_title
;
 Syntheses and structures of four new mixed-amide phosphoric triamides.
;
_journal_coeditor_code           FP3025
_journal_issue                   'Pt 3'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              251
_journal_page_last               259
_journal_paper_doi               10.1107/S2053229616001595
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C17 H36 N3 O1 P1'
_chemical_formula_moiety         'C17 H36 N3 O1 P1'
_chemical_formula_sum            'C17 H36 N3 O P'
_chemical_formula_weight         329.45
_chemical_name_systematic
'<i>rac</i>-<i>N</i>-<i>tert</i>-Butyl-<i>N</i>',<i>N</i>''-dicyclohexyl-<i>N</i>''-methylphosphoric triamide'
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                90
_cell_angle_beta                 90.542(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.9879(4)
_cell_length_b                   19.1972(6)
_cell_length_c                   17.0720(6)
_cell_measurement_reflns_used    12452
_cell_measurement_temperature    175
_cell_measurement_theta_max      27.1970
_cell_measurement_theta_min      1.7090
_cell_volume                     3928.7(2)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_collection
;
GEMINI (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2011)
;
_computing_molecular_graphics
;
<i>PLATON</i> (Spek, 2009) and
<i>Mercury</i> (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
<i>CRYSTALS</i> (Betteridge <i>et al.</i>,  2003) and
<i>enCIFer</i> (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      175
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43414
_diffrn_reflns_theta_full        25.196
_diffrn_reflns_theta_max         29.297
_diffrn_reflns_theta_min         1.596
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2011)
;
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1456.000
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.77
_refine_diff_density_min         -0.83
_refine_ls_abs_structure_details
;
Flack (1983), 9230 Friedel pairs
;
_refine_ls_abs_structure_Flack   -0.08(10)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0883
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         17831
_refine_ls_number_restraints     141
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0960
_refine_ls_shift/su_max          0.0091943
_refine_ls_shift/su_mean         0.0002136
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 419. 494. 196.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1199
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                14523
_reflns_number_total             18366
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            fp3025sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        3928.67(14)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C17 H36 N3 O1 P1'
_cod_database_code               2311850