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_2312350
_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, 0.1C H2 Cl2'
_chemical_formula_moiety         'C29 H25 N O4, 0.1(C H2 Cl2)'
_chemical_formula_sum            'C29.1 H25.2 Cl0.2 N O4'
_chemical_formula_weight         459.99
_chemical_name_systematic
;
<i>N</i>-Triphenylacetyl-<i>L</i>-tyrosine dichloromethane 0.1-solvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_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                   9.28862(9)
_cell_length_b                   10.34013(9)
_cell_length_c                   24.3525(2)
_cell_measurement_reflns_used    19362
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      76.1150
_cell_measurement_theta_min      3.5960
_cell_volume                     2338.95(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0244
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30278
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         4.646
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2021)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             969
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.128
_refine_diff_density_min         -0.143
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1770 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         4276
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+0.3540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                4225
_reflns_number_total             4276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ef3022sup1.cif
_cod_data_source_block           IV
_cod_original_formula_sum        'C29.10 H25.20 Cl0.20 N O4'
_cod_database_code               2312350
_shelx_estimated_absorpt_t_min   0.840
_shelx_estimated_absorpt_t_max   0.973
_shelx_hkl_checksum              20840
_shelx_res_checksum              12829
_cod_database_fobs_code 2312350