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_2311851
_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_moiety         'C20 H34 N3 O P'
_chemical_formula_sum            'C20 H34 N3 O P'
_chemical_formula_weight         363.47
_chemical_name_systematic
'<i>rac</i>-<i>N</i>,<i>N</i>'-Dicyclohexyl-<i>N</i>'-methyl-<i>N</i>''-(<i>p</i>-tolyl)phosphoric triamide'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 98.980(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   10.9207(4)
_cell_length_b                   24.0557(7)
_cell_length_c                   24.3993(8)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    175
_cell_measurement_theta_max      29.0480
_cell_measurement_theta_min      1.9340
_cell_volume                     6331.3(4)
_computing_cell_refinement
;
<i>CrysAlis PRO</i> (Agilent, 2011)
;
_computing_data_collection
;
<i>CrysAlis PRO</i> (Agilent, 2011)
;
_computing_data_reduction
;
<i>CrysAlis PRO</i> (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
;
<i>CRYSTALS</i> (Betteridge <i>et al.</i>,  2003)
;
_computing_structure_solution
;
<i>SUPERFLIP</i> (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      175
_diffrn_detector_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Agilent Xcalibur (Sapphire3, Gemini)'
_diffrn_measurement_method       '\w scans'
_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  0.047
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            44340
_diffrn_reflns_theta_full        25.300
_diffrn_reflns_theta_max         29.102
_diffrn_reflns_theta_min         1.693
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2011)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.320
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         13613
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.0010808
_refine_ls_shift/su_mean         0.0000334
_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:
 0.275E+04 0.448E+04 0.294E+04 0.134E+04 368.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1577
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1515
_reflns_number_gt                10640
_reflns_number_total             14733
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            fp3025sup1.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               2311851