Synthesis and crystal structures of two structurally related kryptoracemates
Kramer, Philipp; Bolte, Michael; Acta Crystallographica Section C 73 (2017) 575–581; doi:10.1107/S2053229617009408

data_2020807
_publ_section_title
;
 Synthesis and crystal structures of two structurally related
 kryptoracemates
;
_journal_coeditor_code           SK3660
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              575
_journal_page_last               581
_journal_paper_doi               10.1107/S2053229617009408
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C25 H28 N2 O3, 0.5C H2 Cl2'
_chemical_formula_moiety         'C25 H28 N2 O3, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C25.5 H29 Cl N2 O3'
_chemical_formula_weight         446.96
_chemical_name_systematic
;<i>rac</i>-<i>N</i>-[(1<i>S</i>,2<i>S</i>,3<i>R</i>)-2-Methyl-3-(5-methylfuran-2-yl)-1-phenyl-3-(propionamido)propyl]benzamide dichloromethane
hemisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                109.248(8)
_cell_angle_beta                 97.929(9)
_cell_angle_gamma                91.214(8)
_cell_formula_units_Z            4
_cell_length_a                   10.1501(11)
_cell_length_b                   14.8556(15)
_cell_length_c                   17.662(2)
_cell_measurement_reflns_used    16955
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.86
_cell_measurement_theta_min      3.41
_cell_volume                     2483.9(5)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2001)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2001)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2001)
;
_computing_molecular_graphics
;
XP (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe IPDS II two-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19477
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         3.430
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(X-AREA; Stoe & Cie, 2001)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       needle
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.456
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2795 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1163
_refine_ls_number_reflns         14382
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0789
_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^)+(0.0968P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1815
_refine_ls_wR_factor_ref         0.1952
_reflns_number_gt                9998
_reflns_number_total             14382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3660sup1.cif
_cod_data_source_block           II
_cod_original_formula_sum        'C25.5 H29 Cl1 N2 O3'
_cod_database_code               2020807
_cod_database_fobs_code          2020807
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.977
_shelx_hkl_checksum              14905
_shelx_res_checksum              20529