Crystal structure of tert-butyl (1S,2R,5R)-2-(hydroxymethyl)-4-(4-methoxyphenyl)-6-oxa-3-azabicyclo[3.1.0]hexane-3-carboxylate, C17H23NO5
Caracelli, Ignez; Zukerman-Schpector, Julio; Garcia, Ariel L. Llanes; Correia, Carlos Roque D.; Tiekink, Edward R.T.; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1431–1433; doi:10.1515/ncrs-2020-0349

data_8105486
_publ_section_title
;
 Crystal structure of tert-butyl
 (1S,2R,5R)-2-(hydroxymethyl)-4-(4-methoxyphenyl)-6-oxa-3-azabicyclo[3.1.0]hexane-3-carboxylate,
 C17H23NO5
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1431
_journal_page_last               1433
_journal_paper_doi               10.1515/ncrs-2020-0349
_journal_volume                  235
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C17 H23 N O5'
_chemical_formula_sum            'C17 H23 N O5'
_chemical_formula_weight         321.36
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 94.174(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.0479(9)
_cell_length_b                   9.7032(10)
_cell_length_c                   14.711(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.12
_cell_measurement_theta_min      9.89
_cell_volume                     861.0(2)
_computing_cell_refinement       'XCAD4 [2]'
_computing_data_collection       'CAD4 Express [1]'
_computing_data_reduction        'XCAD4 [2]'
_computing_molecular_graphics    'ORTEP-3 for Windows [5]'
_computing_publication_material  'SHELXL-2018/3 [4]'
_computing_structure_refinement  'SHELXL-2018/3 [4]'
_computing_structure_solution    'SIR2014 [3]'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled \w/2\q scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0805
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            2373
_diffrn_reflns_point_group_measured_fraction_full 0.531
_diffrn_reflns_point_group_measured_fraction_max 0.527
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.969
_diffrn_reflns_theta_min         1.388
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        1.1
_diffrn_standards_interval_time  30
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       irregular
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2177
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0865P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                959
_reflns_number_total             2177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0349_suppl.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               8105486
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.993