Dimethoxyphosphinoyl phenyl ketone <i>p</i>-tolylsulfonylhydrazone
Demoin, Dustin Wayne; Pluth, Michael; Soo, Han Sen; Xu, Yue; Acta Crystallographica Section E 62 (2006) o3551–o3552; doi:10.1107/S1600536806025451

data_2209750
_publ_section_title
;
 Dimethoxyphosphinoyl phenyl ketone <i>p</i>-tolylsulfonylhydrazone
;
_journal_coeditor_code           BI2025
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3551
_journal_page_last               o3552
_journal_paper_doi               10.1107/S1600536806025451
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C16 H19 N2 O5 P S'
_chemical_formula_moiety         'C16 H19 N2 O5 P S'
_chemical_formula_sum            'C16 H19 N2 O5 P S'
_chemical_formula_weight         382.36
_chemical_name_common
;
Dimethoxyphosphinoyl phenyl ketone <i>p</i>-tolylsulfonylhydrazone
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 92.514(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4692(19)
_cell_length_b                   10.889(3)
_cell_length_c                   9.690(2)
_cell_measurement_reflns_used    1816
_cell_measurement_temperature    166.0(10)
_cell_measurement_theta_max      21.4
_cell_measurement_theta_min      2.8
_cell_volume                     892.8(4)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      166.0(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4987
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.294
_refine_ls_abs_structure_details 'Flack (1983), 971 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.05(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         2788
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                2383
_reflns_number_total             2788
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi2025.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               2209750
_cod_database_fobs_code          2209750