The crystal structure of tert-butyl 2-(4-(12-bromo [2.2]paracyclophanyl)carbamoyl)pyrrolidine-1-carboxylate, C26H31BrN2O3
Zhen, Chen; Yanwen, Sun; Yingying, Meng; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 1185–1187; doi:10.1515/ncrs-2022-0458

data_8107329
_publ_section_title
;
 The crystal structure of tert-butyl 2-(4-(12-bromo
 [2.2]paracyclophanyl)carbamoyl)pyrrolidine-1-carboxylate, C26H31BrN2O3
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1185
_journal_page_last               1187
_journal_paper_doi               10.1515/ncrs-2022-0458
_journal_volume                  237
_journal_year                    2022
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C26 H31 Br N2 O3'
_chemical_formula_sum            'C26 H31 Br N2 O3'
_chemical_formula_weight         499.44
_chemical_name_systematic
;  
tert-butyl 2-(4-(12-bromo [2.2] Paracyclophanyl)
carbamoyl) pyrrolidine-1-carboxylate
;
_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     direct
_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                   11.010(10)
_cell_length_b                   13.227(12)
_cell_length_c                   16.458(14)
_cell_measurement_reflns_used    3504
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.648
_cell_measurement_theta_min      2.703
_cell_volume                     2397(4)
_computing_cell_refinement       'Bruker [1]'
_computing_data_reduction        'Bruker [1]'
_computing_molecular_graphics    'DIAMOND [5]'
_computing_publication_material  'ShelXL [4]'
_computing_structure_refinement  'ShelXL [4]'
_computing_structure_solution    'OLEX2 [2], ShelXS [3]'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17705
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.676
_diffrn_reflns_theta_min         2.707
_exptl_absorpt_coefficient_mu    1.745
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 1225 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0225P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                3657
_reflns_number_total             5536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0458_suppl.cif
_cod_data_source_block           p
_cod_database_code               8107329
_shelx_estimated_absorpt_t_max   0.845
_shelx_estimated_absorpt_t_min   0.722
_shelx_res_checksum              6846
_shelx_hkl_checksum              81318