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_2311853
_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          'C12 H26 N3 O P'
_chemical_formula_moiety         'C12 H26 N3 O P'
_chemical_formula_sum            'C12 H26 N3 O P'
_chemical_formula_weight         259.33
_chemical_name_systematic
;
2-[Cyclohexyl(methyl)amino]-5,5-dimethyl-1,3,2\l^5^-diazaphosphinan-2-one
;
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.3318(3)
_cell_length_b                   10.3065(5)
_cell_length_c                   23.1616(10)
_cell_measurement_reflns_used    4337
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.7460
_cell_measurement_theta_min      2.1670
_cell_volume                     1511.50(12)
_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 0.984
_diffrn_measured_fraction_theta_max 0.922
_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  0.071
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13647
_diffrn_reflns_theta_full        25.277
_diffrn_reflns_theta_max         29.054
_diffrn_reflns_theta_min         1.758
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2011)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.36
_refine_ls_abs_structure_details 'Flack (1983), 1519 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.03(16)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9665
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3625
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.0089624
_refine_ls_shift/su_mean         0.0014744
_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:
 0.167E+04 0.247E+04 0.143E+04 638. 36.7
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1244
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1207
_reflns_number_gt                2989
_reflns_number_total             3678
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            fp3025sup1.cif
_cod_data_source_block           IV
_cod_original_cell_volume        1511.48(13)
_cod_database_code               2311853