Synthesis and crystal structure of a novel prochiral ketoimine: (E)-acetophenoneO-diphenylphosphoryl oxime
Majer, Sean H.; Tanski, Joseph M.; Acta Crystallographica Section C Structural Chemistry 71 (2015) –; doi:10.1107/S2053229615002351

data_2019843
_publ_section_title
;
 Synthesis and crystal structure of a novel prochiral ketoimine:
 (E)-acetophenoneO-diphenylphosphoryl oxime
;
_journal_coeditor_code           LF3007
_journal_issue                   3
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229615002351
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C20 H18 N O2 P'
_chemical_formula_moiety         'C20 H18 N O2 P'
_chemical_formula_sum            'C20 H18 N O2 P'
_chemical_formula_weight         335.32
_chemical_name_systematic
;
(<i>E</i>)-Acetophenone <i>O</i>-diphenylphosphoryl oxime
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 105.133(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.035(2)
_cell_length_b                   5.9874(7)
_cell_length_c                   16.236(2)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    125.(2)
_cell_measurement_theta_max      71.2433
_cell_measurement_theta_min      5.0810
_cell_volume                     1692.4(3)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEXII (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL2014 (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL2014 (Sheldrick, 2008), Mercury (Macrae <i>et al.</i>,
2008) and
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXTL2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      125.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'Cu IuS micro-focus source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21556
_diffrn_reflns_theta_full        66.57
_diffrn_reflns_theta_max         66.57
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.414
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.8622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0912
_reflns_number_gt                2928
_reflns_number_total             2983
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lf3007sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1692.4(4)
_cod_database_code               2019843
_cod_database_fobs_code          2019843
_shelx_hkl_checksum              6732
_shelx_res_checksum              56910