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_2312347
_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, C1 H1 Cl3'
_chemical_formula_moiety         'C29 H25 N O4, C1 H1 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      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 109.945(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0732(3)
_cell_length_b                   10.0051(2)
_cell_length_c                   14.7474(4)
_cell_measurement_reflns_used    17066
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      75.4280
_cell_measurement_theta_min      3.1280
_cell_volume                     1397.15(7)
_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 10.5357
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0496
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18782
_diffrn_reflns_theta_full        66.575
_diffrn_reflns_theta_max         66.575
_diffrn_reflns_theta_min         3.188
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2021)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       needle
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.413
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2221 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.003(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         4905
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+0.5933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                4842
_reflns_number_total             4905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ef3022sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1397.14(6)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2312347
_shelx_estimated_absorpt_t_min   0.533
_shelx_estimated_absorpt_t_max   0.908
_shelx_hkl_checksum              75565
_shelx_res_checksum              88543
_cod_database_fobs_code 2312347