A diversity-oriented synthesis of cyclopenta[b]pyrroles and related compounds through a calcium(ii)/copper(ii) catalytic sequence
Marin, L.; Guillot, R.; Gandon, V.; Schulz, E.; Lebœuf, D.; Organic Chemistry Frontiers 5 (2018) 640–; doi:10.1039/C7QO00948H

data_1553944
_publ_section_title
;
 A diversity-oriented synthesis of cyclopenta[b]pyrroles and related
 compounds through a calcium(ii)/copper(ii) catalytic sequence
;
_journal_issue                   4
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              640
_journal_paper_doi               10.1039/C7QO00948H
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C33 H27 N O3, C H2 Cl2 '
_chemical_formula_sum            'C34 H29 Cl2 N O3'
_chemical_formula_weight         570.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-06-13 deposited with the CCDC.
2017-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.282(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1223(5)
_cell_length_b                   10.4359(3)
_cell_length_c                   19.4476(6)
_cell_measurement_reflns_used    5626
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.22
_cell_volume                     2843.05(16)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36151
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.566
_diffrn_reflns_theta_min         2.111
_exptl_absorpt_coefficient_mu    0.265
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         8452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.185
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.9585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1434
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5090
_reflns_number_total             8452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qo00948h2.cif
_cod_data_source_block           8ac
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1553944
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              4653
_shelx_hkl_checksum              66402