Hydrogen bonding-promoted tunable approach for access to aza-bicyclo-[3.3.0]octanes and cyclopenta[<i>b</i>] pyrroles.
Pramanik, Sourav; Hazra, Subhadeep; Chatterjee, Ayan; Saha, Jaideep; Chemical communications (Cambridge, England) 60 (2024) 4922–4925; doi:10.1039/d4cc01065e

data_7132917
_publ_section_title
;
 Hydrogen bonding-promoted tunable approach for access to
 aza-bicyclo-[3.3.0]octanes and cyclopenta[<i>b</i>] pyrroles.
;
_journal_issue                   37
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4922
_journal_page_last               4925
_journal_paper_doi               10.1039/d4cc01065e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C31 H29 N O5'
_chemical_formula_sum            'C31 H29 N O5'
_chemical_formula_weight         495.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-02-07 deposited with the CCDC.	2024-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                101.529(3)
_cell_angle_beta                 90.637(3)
_cell_angle_gamma                113.153(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8447(8)
_cell_length_b                   11.1980(8)
_cell_length_c                   12.0881(10)
_cell_measurement_reflns_used    6789
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.81
_cell_volume                     1315.93(18)
_computing_cell_refinement       'APEX4 V8.40B (Bruker, 2021)'
_computing_data_collection       'APEX4 (Bruker, v2021.4-0)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2021)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 2012) '
_computing_publication_material  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker D8 VENTURE diffractometer equipped with PHOTON II detector'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            42149
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         3.457
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2016/2 - Bruker AXS area detector scaling and absorption 
 correction
 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4884
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.8131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3229
_reflns_number_total             4884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01065e2.cif
_cod_data_source_block           SP-1162
_cod_depositor_comments          'Adding full bibliography for 7132917.cif.'
_cod_database_code               7132917
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              31773
_shelx_hkl_checksum              59186