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_1555588
_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 H49 Cu N6 O2, 0.59(C H Cl3)'
_chemical_formula_sum            'C53.59 H49.59 Cl1.77 Cu N6 O2'
_chemical_formula_weight         935.95
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.850(5)
_cell_angle_beta                 78.821(5)
_cell_angle_gamma                77.371(5)
_cell_formula_units_Z            2
_cell_length_a                   8.0804(6)
_cell_length_b                   16.5626(10)
_cell_length_c                   17.4337(11)
_cell_measurement_reflns_used    777
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      42.36
_cell_measurement_theta_min      2.74
_cell_volume                     2225.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_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 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.1419
_diffrn_reflns_av_sigmaI/netI    0.2387
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13801
_diffrn_reflns_theta_full        58.92
_diffrn_reflns_theta_max         58.92
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    2.068
_exptl_absorpt_correction_T_max  0.9796
_exptl_absorpt_correction_T_min  0.6938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
The 
69 electrons removed by SQUEEZE correspond to 1.18 molecules of
disordered chloroform per unit cell, or 0.59 per corrole molecule.
The disordered solvent is included in the formula, FW, density,
etc., but is not in the model.
;
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         6179
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.1867
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1861
_reflns_number_gt                2544
_reflns_number_total             6179
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ol6b01314_si_002.cif
_cod_data_source_block           BBB3-2015
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1   '
_cod_database_code               1555588