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_7154960
_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         'C55 H53 Cu N6, 1.95(C H Cl3)'
_chemical_formula_sum            'C56.95 H54.95 Cl5.85 Cu N6'
_chemical_formula_weight         1094.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 91.878(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7796(8)
_cell_length_b                   31.6279(17)
_cell_length_c                   11.1541(5)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      65.94
_cell_measurement_theta_min      2.79
_cell_volume                     5211.2(5)
_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      100.0(5)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_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  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            43548
_diffrn_reflns_theta_full        66.55
_diffrn_reflns_theta_max         66.55
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    3.697
_exptl_absorpt_correction_T_max  0.8662
_exptl_absorpt_correction_T_min  0.5940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2268
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform/methanol'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
The 220 electrons removed by SQUEEZE correspond to 3.8 molecules
of disordered chloroform per unit cell or 0.95 per corrole complex.
The disordered solvent, along with the ordered solvent is included in
the formula, FW, etc., but is not included in the model.
;
_refine_diff_density_max         0.971
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         8298
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0948
_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^)+(0.1151P)^2^+33.6771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2453
_refine_ls_wR_factor_ref         0.2624
_reflns_number_gt                6186
_reflns_number_total             8298
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5ob02572a2.cif
_cod_data_source_block           Compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21/c  '
_cod_database_code               7154960