Crystal structure of (3,5-dimethyl-1<i>H</i>-pyrrol-2-yl)diphenylphosphine oxide
Kang, Sung Kwon; Choi, Eung Man; Son, Kyung-sun; Acta Crystallographica Section E 73 (2017) 1268–1270; doi:10.1107/S2056989017010994

data_2242266
_publ_section_title
;
 Crystal structure of
 (3,5-dimethyl-1<i>H</i>-pyrrol-2-yl)diphenylphosphine oxide
;
_journal_coeditor_code           WM5405
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1268
_journal_page_last               1270
_journal_paper_doi               10.1107/S2056989017010994
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C18 H18 N O P'
_chemical_formula_moiety         'C18 H18 N O P'
_chemical_formula_sum            'C18 H18 N O P'
_chemical_formula_weight         295.30
_chemical_name_systematic
;
(3,5-Dimethyl-1<i>H</i>-pyrrol-2-yl)diphenylphosphine
oxide
;
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.378(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.656(6)
_cell_length_b                   14.765(8)
_cell_length_c                   20.757(11)
_cell_measurement_reflns_used    6973
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.37
_cell_volume                     3231(3)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14781
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.441
_diffrn_reflns_theta_min         1.983
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0690P)^2^+1.3679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1358
_reflns_number_gt                3196
_reflns_number_total             3961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5405sup1.cif
_cod_data_source_block           I
_cod_database_code               2242266
_cod_database_fobs_code          2242266
_shelx_hkl_checksum              81629
_shelx_res_checksum              84940