Diethyl (1-benzyl-4-phenyl-3-trifluoromethyl-1<i>H</i>-pyrrol-2-yl)phosphonate
Jezuita, Anna; Cal, Dariusz; Zagórski, Piotr; Ejsmont, Krzysztof; Zarychta, Bartosz; IUCrData 2 (2017) x171122–; doi:10.1107/S2414314617011221

data_1546773
_publ_section_title
;
 Diethyl
 (1-benzyl-4-phenyl-3-trifluoromethyl-1<i>H</i>-pyrrol-2-yl)phosphonate
;
_journal_coeditor_code           HB4162
_journal_issue                   8
_journal_name_full               IUCrData
_journal_page_first              x171122
_journal_paper_doi               10.1107/S2414314617011221
_journal_volume                  2
_journal_year                    2017
_chemical_formula_iupac          'C22 H23 F3 N O3 P'
_chemical_formula_moiety         'C22 H23 F3 N O3 P'
_chemical_formula_sum            'C22 H23 F3 N O3 P'
_chemical_formula_weight         437.38
_chemical_name_systematic
;
Diethyl (1-benzyl-4-phenyl-3-trifluoromethyl-1<i>H</i>-pyrrol-2-yl)phosphonate
;
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.744(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7056(3)
_cell_length_b                   10.6494(2)
_cell_length_c                   14.9163(3)
_cell_measurement_reflns_used    14420
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.999
_cell_measurement_theta_min      2.974
_cell_volume                     2176.12(8)
_computing_cell_refinement
;
CrysAlisCCD (Oxford Diffraction, 2008)
;
_computing_data_collection
;
CrysAlisCCD (Oxford Diffraction, 2008)
;
_computing_data_reduction
;
CrysAlisCCD (Oxford Diffraction, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean '1024 x 1024 with blocks 2 x 2'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14420
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.974
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.305
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0481P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                3251
_reflns_number_total             4254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb4162sup1.cif
_cod_data_source_block           I
_cod_database_code               1546773
_cod_database_fobs_code          1546773
_shelx_hkl_checksum              85997
_shelx_res_checksum              79986
_shelxl_version_number           .2013