β-Pyrrolopyrazino Annulated Corroles via a Pictet-Spengler Approach.
Berionni Berna, Beatrice; Nardis, Sara; Galloni, Pierluca; Savoldelli, Andrea; Stefanelli, Manuela; Fronczek, Frank R.; Smith, Kevin M.; Paolesse, Roberto; Organic letters 18 (2016) 3318–3321; doi:10.1021/acs.orglett.6b01314

data_1555589
_publ_section_title
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 \b-Pyrrolopyrazino Annulated Corroles via a Pictet-Spengler Approach.
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_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3318
_journal_page_last               3321
_journal_paper_doi               10.1021/acs.orglett.6b01314
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C53 H51 Cu N6, C H Cl3 '
_chemical_formula_sum            'C54 H52 Cl3 Cu N6'
_chemical_formula_weight         954.90
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 113.596(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0310(11)
_cell_length_b                   30.509(3)
_cell_length_c                   13.9111(9)
_cell_measurement_reflns_used    5114
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      63.20
_cell_measurement_theta_min      2.90
_cell_volume                     4679.2(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker Kappa APEX-II DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer optics'
_diffrn_radiation_source         'I\mS microfocus'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.1567
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28056
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.358
_diffrn_reflns_theta_min         2.897
_exptl_absorpt_coefficient_mu    2.574
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       needle
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         8213
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1866
_refine_ls_R_factor_gt           0.0810
_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^)+(0.0942P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1779
_refine_ls_wR_factor_ref         0.2270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3744
_reflns_number_total             8213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b01314_si_002.cif
_cod_data_source_block           BBB1-2016
_cod_original_cell_volume        4679.3(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1555589
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.627
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              38010
_shelx_hkl_checksum              82274