Crystal structures of 1-(4-chlorophenyl)-2-(diphenylphosphoryl)ethan-1-one and 1-(diphenylphosphoryl)-3,3-dimethylbutan-2-one
Leach, Erin G.; Kulesza, Alyssa A.; Staples, Richard J.; Biros, Shannon M.; Acta Crystallographica Section E 71 (2015) 523–527; doi:10.1107/S2056989015006994

data_2240623
_publ_section_title
;
 Crystal structures of
 1-(4-chlorophenyl)-2-(diphenylphosphoryl)ethan-1-one and
 1-(diphenylphosphoryl)-3,3-dimethylbutan-2-one
;
_journal_coeditor_code           SU5111
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              523
_journal_page_last               527
_journal_paper_doi               10.1107/S2056989015006994
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C20 H16 Cl O2 P'
_chemical_formula_moiety         'C20 H16 Cl O2 P'
_chemical_formula_sum            'C20 H16 Cl O2 P'
_chemical_formula_weight         354.75
_chemical_name_systematic
;
1-(4-Chlorophenyl)-2-(diphenylphosphoryl)ethan-1-one
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3107 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.7380(2)
_cell_length_b                   14.4453(3)
_cell_length_c                   19.9515(3)
_cell_measurement_reflns_used    9053
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.006
_cell_measurement_theta_min      4.432
_cell_volume                     3382.96(10)
_computing_cell_refinement
;
APEX2 and SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT and XPREP (Bruker, 2013)
;
_computing_molecular_graphics
;
CrystalMaker (Palmer, 2007)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009; Bourhis <i>et al.</i>,
2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      172.99
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17900
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.176
_diffrn_reflns_theta_min         4.432
_exptl_absorpt_coefficient_mu    2.965
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.5990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       needle
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.388
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0502P)^2^+1.0258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0894
_reflns_number_gt                2880
_reflns_number_total             3297
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su5111sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        3382.95(10)
_cod_database_code               2240623
_cod_database_fobs_code          2240623
_shelx_estimated_absorpt_t_min   0.418
_shelx_estimated_absorpt_t_max   0.699
_shelxl_version_number           2.014