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_1555590
_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         'C54 H40 Cu N6, 1.5(C H Cl3)'
_chemical_formula_sum            'C55.5 H50.5 Cl4.5 Cu N6'
_chemical_formula_weight         1024.58
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           Monoclinic'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 98.807(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.4929(11)
_cell_length_b                   11.6131(5)
_cell_length_c                   33.0447(14)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      28.90
_cell_measurement_theta_min      2.37
_cell_volume                     9667.6(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEX-II DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            68359
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.61
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  0.8836
_exptl_absorpt_correction_T_min  0.8066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.324
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         13528
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+54.0407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.1814
_reflns_number_gt                11304
_reflns_number_total             13528
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ol6b01314_si_002.cif
_cod_data_source_block           BBB3-2016
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C55.50 H50.50 Cl4.50 Cu N6'
_cod_database_code               1555590