Diversity of N-triphenylacetyl-L-tyrosine solvates with halogenated solvents.
Czapik, Agnieszka; Kwit, Marcin; Acta crystallographica. Section C, Structural chemistry 77 (2021) 745–756; doi:10.1107/S2053229621011098

data_2312349
_publ_section_title
;
 Diversity of N-triphenylacetyl-L-tyrosine solvates with halogenated
 solvents.
;
_journal_coeditor_code           EF3022
_journal_issue                   'Pt 12'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              745
_journal_page_last               756
_journal_paper_doi               10.1107/S2053229621011098
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration rm
_chemical_formula_iupac          'C29 H25 N O4, C H Cl3'
_chemical_formula_moiety         'C29 H25 N O4, C H Cl3'
_chemical_formula_sum            'C30 H26 Cl3 N O4'
_chemical_formula_weight         570.87
_chemical_name_systematic
;
<i>N</i>-Triphenylacetyl-<i>L</i>-tyrosine chloroform monosolvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.27898(12)
_cell_length_b                   32.3574(4)
_cell_length_c                   9.96336(12)
_cell_measurement_reflns_used    16633
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      75.8170
_cell_measurement_theta_min      2.7240
_cell_volume                     2991.44(6)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 10.5384
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Rigaku SuperNova Single Source diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29945
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.424
_diffrn_reflns_theta_min         4.438
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.052
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2021)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       needle
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.266
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2454 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.034(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0408P)^2^+0.7639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                5987
_reflns_number_total             6241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ef3022sup1.cif
_cod_data_source_block           III
_cod_database_code               2312349
_shelx_estimated_absorpt_t_min   0.415
_shelx_estimated_absorpt_t_max   0.970
_shelx_hkl_checksum              97785
_shelx_res_checksum              27910
_shelx_fab_checksum              65294
_cod_database_fobs_code 2312349