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_2240624
_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          'C18 H21 O2 P'
_chemical_formula_moiety         'C18 H21 O2 P'
_chemical_formula_sum            'C18 H21 O2 P'
_chemical_formula_weight         300.32
_chemical_name_systematic
;
1-(Diphenylphosphoryl)-3,3-dimethylbutan-2-one
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 112.2120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3416(2)
_cell_length_b                   10.5161(2)
_cell_length_c                   10.2790(2)
_cell_measurement_reflns_used    5567
_cell_measurement_temperature    173
_cell_measurement_theta_max      71.991
_cell_measurement_theta_min      4.646
_cell_volume                     834.77(3)
_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      173.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7043
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.984
_diffrn_reflns_theta_min         4.647
_exptl_absorpt_coefficient_mu    1.466
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.6307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       needle
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.383
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1090 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.088(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3006
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0722P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                2774
_reflns_number_total             3006
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su5111sup1.cif
_cod_data_source_block           II
_cod_database_code               2240624
_cod_database_fobs_code          2240624
_shelx_estimated_absorpt_t_min   0.570
_shelx_estimated_absorpt_t_max   0.887