Structural reasons for the formation of multicomponent products and the influence of high pressure
Konieczny, Krzysztof A.; Bakowicz, Julia; Paliwoda, Damian; Warren, Mark R.; Ciesielski, Arkadiusz; Cyrański, Michał K.; Turowska-Tyrk, Ilona; Acta Crystallographica Section B 77 (2021) –; doi:10.1107/S2052520621004492

data_2108817
_publ_section_title
;
 Structural reasons for the formation of multicomponent products and the
 influence of high pressure
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520621004492
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration syn
_chemical_formula_sum            'C31 H39 N O3'
_chemical_formula_weight         473.63
_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   geom
_atom_sites_solution_primary     isomor
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.9793(10)
_cell_length_b                   13.334(4)
_cell_length_c                   31.884(8)
_cell_measurement_pressure       750000
_cell_measurement_reflns_used    2531
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      23.8
_cell_measurement_theta_min      2.4
_cell_volume                     2542.0(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2008)'
_diffrn_ambient_pressure         750000
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.516
_diffrn_measured_fraction_theta_max 0.511
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f- and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70932
_diffrn_reflns_av_R_equivalents  0.1317
_diffrn_reflns_av_unetI/netI     0.1466
_diffrn_reflns_Laue_measured_fraction_full 0.516
_diffrn_reflns_Laue_measured_fraction_max 0.511
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            13624
_diffrn_reflns_point_group_measured_fraction_full 0.515
_diffrn_reflns_point_group_measured_fraction_max 0.509
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.383
_diffrn_reflns_theta_min         1.655
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
The absolute configuration was assigned to agree with that of its
precursor (S)-(-)-1-phenylethaneamine at the chiral centre C25.
;
_refine_ls_abs_structure_Flack   -0.9(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         2378
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1729
_refine_ls_R_factor_gt           0.0691
_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^)+(0.0914P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1886
_reflns_Friedel_coverage         0.713
_reflns_Friedel_fraction_full    0.514
_reflns_Friedel_fraction_max     0.507
_reflns_number_gt                1201
_reflns_number_total             2378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eb5068sup1.cif
_cod_data_source_block           10hUV_075GPa
_cod_database_code               2108817
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.969
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              67191
_shelx_hkl_checksum              32932
_cod_database_fobs_code 2108817