Extending the corrole ring conjugation: preparation of β,β'-fused 2,3-[1',2'-b]pyrazinocorroles.
Berionni Berna, Beatrice; Nardis, Sara; Mandoj, Federica; Fronczek, Frank R.; Smith, Kevin M.; Paolesse, Roberto; Organic & biomolecular chemistry 14 (2016) 2891–2897; doi:10.1039/c5ob02572a

data_7154962
_publ_section_title
;
 Extending the corrole ring conjugation: preparation of \b,\b'-fused
 2,3-[1',2'-b]pyrazinocorroles.
;
_journal_issue                   10
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2891
_journal_page_last               2897
_journal_paper_doi               10.1039/c5ob02572a
_journal_volume                  14
_journal_year                    2016
_chemical_formula_moiety         'C63 H53 Cu N6, C H Cl3, 1.39(C H4 O)'
_chemical_formula_sum            'C65.39 H59.56 Cl3 Cu N6 O1.39'
_chemical_formula_weight         1121.56
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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
_audit_update_record
;
2015-11-18 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                115.779(2)
_cell_angle_beta                 95.558(2)
_cell_angle_gamma                104.159(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7135(5)
_cell_length_b                   15.8594(6)
_cell_length_c                   15.8605(6)
_cell_measurement_reflns_used    7266
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.49
_cell_volume                     2715.49(19)
_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 0.997
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31555
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.9648
_exptl_absorpt_correction_T_min  0.7976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1170
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/chloroform'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
The 50 electrons removed by SQUEEZE correspond to 2.78
molecules of disordered methanol per unit cell, or 1.39
per corrole molecule. This solvent is included in the
formula, FW, density, etc., but is not in the model.
;
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         12906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0956P)^2^+0.5685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                9356
_reflns_number_total             12906
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5ob02572a2.cif
_cod_data_source_block           Compound8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7154960--7154962.cif.
;
_cod_original_cell_volume        2715.48(18)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1   '
_cod_database_code               7154962