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_2019739
_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          'C10 H17 N2 O2 P1 S1'
_chemical_formula_moiety         'C10 H17 N2 O2 P1 S1'
_chemical_formula_sum            'C10 H17 N2 O2 P S'
_chemical_formula_weight         260.3
_chemical_name_systematic
;
<i>O</i>,<i>O</i>'-Diethyl (2-phenylhydrazin-1-yl)thiophosphonate
;
_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                 104.553(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9380(10)
_cell_length_b                   16.3798(10)
_cell_length_c                   8.4156(6)
_cell_measurement_reflns_used    4151
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.79
_cell_volume                     1325.96(19)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2012)
;
_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
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.91
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur Atlas Gemini ultra'
_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     0.7107
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0154
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9959
_diffrn_reflns_theta_full        27.34
_diffrn_reflns_theta_max         28.41
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.3035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.717
_exptl_crystal_size_mid          0.496
_exptl_crystal_size_min          0.239
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.78
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    95
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3038
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.0199
_refine_ls_shift/su_mean         0.0009
_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          0.1009
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                2628
_reflns_number_total             3038
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            fg3325sup1.cif
_cod_data_source_block           II
_cod_original_sg_symbol_Hall     '-P 2ycb'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C10 H17 N2 O2 P1 S1'
_cod_database_code               2019739
_cod_database_fobs_code          2019739