Crystal structure of bis(3,3-dimethyl-2-oxobutyl)diphenylphosphonium bromide chloroform monosolvate
Kulesza, Alyssa A.; Staples, Richard J.; Biros, Shannon M.; Acta Crystallographica Section E 71 (2015) o339–o340; doi:10.1107/S205698901500763X

data_2240637
_publ_section_title
;
 Crystal structure of bis(3,3-dimethyl-2-oxobutyl)diphenylphosphonium
 bromide chloroform monosolvate
;
_journal_coeditor_code           PK2549
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o339
_journal_page_last               o340
_journal_paper_doi               10.1107/S205698901500763X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C24 H32 O2 P +, Br -, C H Cl3'
_chemical_formula_moiety         'C24 H32 O2 P +, Br -, C H Cl3'
_chemical_formula_sum            'C25 H33 Br Cl3 O2 P'
_chemical_formula_weight         582.74
_chemical_name_systematic
;
Bis(3,3-dimethyl-2-oxobutyl)diphenylphosphonium bromide
chloroform monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.7020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.6380(18)
_cell_length_b                   13.6273(10)
_cell_length_c                   18.1817(13)
_cell_measurement_reflns_used    9180
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.319
_cell_measurement_theta_min      2.269
_cell_volume                     5547.5(7)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (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      173.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25767
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.749
_exptl_absorpt_coefficient_mu    1.848
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       plate
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.302
_refine_diff_density_min         -1.095
_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     373
_refine_ls_number_reflns         5090
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0643
_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^)+(0.1214P)^2^+22.4904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.2062
_reflns_number_gt                3862
_reflns_number_total             5090
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2549sup1.cif
_cod_data_source_block           I
_cod_database_code               2240637
_shelx_estimated_absorpt_t_min   0.569
_shelx_estimated_absorpt_t_max   0.848
_shelx_hkl_checksum              32397
_shelx_res_checksum              80049
_shelxl_version_number           2.014
_cod_database_fobs_code 2240637