Two new thiophosphoramide structures: <i>N</i>,<i>N</i>',<i>N</i>''-tricyclohexylphosphorothioic triamide and <i>O</i>,<i>O</i>'-diethyl (2-phenylhydrazin-1-yl)thiophosphonate
Pourayoubi, Mehrdad; Abrishami, Mozhgan; Eigner, Václav; Nečas, Marek; Dušek, Michal; Delavar, Mahmoud; Acta Crystallographica Section C 70 (2014) –; doi:10.1107/S2053229614022608

data_2019738
_publ_section_title
;
 Two new thiophosphoramide structures:
 <i>N</i>,<i>N</i>',<i>N</i>''-tricyclohexylphosphorothioic triamide and
 <i>O</i>,<i>O</i>'-diethyl (2-phenylhydrazin-1-yl)thiophosphonate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614022608
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C18 H36 N3 P1 S1'
_chemical_formula_moiety         'C18 H36 N3 P1 S1'
_chemical_formula_sum            'C18 H36 N3 P S'
_chemical_formula_weight         357.5
_chemical_name_systematic
;
<i>N</i>,<i>N</i>',<i>N</i>''-Tricyclohexylphosphorothioic triamide
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0897(7)
_cell_length_b                   18.6342(15)
_cell_length_c                   12.2598(8)
_cell_measurement_reflns_used    7402
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.0
_cell_measurement_theta_min      3.1
_cell_volume                     2076.6(3)
_computing_cell_refinement
;
<i>CrystalClear-SM Expert</i> (Rigaku, 2011)
;
_computing_data_collection
;
<i>CrystalClear-SM Expert</i> (Rigaku, 2011)
;
_computing_data_reduction
;
<i>CrystalClear-SM Expert</i> (Rigaku, 2011)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2005) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
enCIFer (Allen <i>et al.</i>, 2004)
;
_computing_structure_refinement
;
<i>JANA2006</i> (Pet\<r\'i\<cek <i>et al.</i>, 2014)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.93
_diffrn_measurement_device
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Multilayer
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18907
_diffrn_reflns_theta_full        31.55
_diffrn_reflns_theta_max         33.05
_diffrn_reflns_theta_min         3.68
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrystalClear-SM Expert</i>; Rigaku, 2011)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.1436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.80
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    71
_refine_ls_number_parameters     117
_refine_ls_number_reflns         3731
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.0088
_refine_ls_shift/su_mean         0.0014
_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          0.1134
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                2645
_reflns_number_total             3731
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            fg3325sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-P -2xabc;-2yb;-2zac'
_cod_original_formula_sum        'C18 H36 N3 P1 S1'
_cod_database_code               2019738
_cod_database_fobs_code          2019738