Formation, structure, and reactivity of meso-tetraaryl-chlorolactones, -porpholactams, and -chlorolactams, porphyrin and chlorin analogues incorporating oxazolone or imidazolone moieties.
Akhigbe, Joshua; Haskoor, John; Krause, Jeanette A.; Zeller, Matthias; Brückner, Christian; Organic & biomolecular chemistry 11 (2013) 3616–3628; doi:10.1039/c3ob40138c

data_7152931
_publ_section_title
;
 Formation, structure, and reactivity of meso-tetraaryl-chlorolactones,
 -porpholactams, and -chlorolactams, porphyrin and chlorin analogues
 incorporating oxazolone or imidazolone moieties.
;
_journal_issue                   22
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3616
_journal_page_last               3628
_journal_paper_doi               10.1039/c3ob40138c
_journal_volume                  11
_journal_year                    2013
_chemical_formula_sum            'C51 H38 F12 N6 O3'
_chemical_formula_weight         1010.87
_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
_cell_angle_alpha                81.419(5)
_cell_angle_beta                 75.271(5)
_cell_angle_gamma                84.415(5)
_cell_formula_units_Z            2
_cell_length_a                   12.801(4)
_cell_length_b                   12.814(4)
_cell_length_c                   14.782(5)
_cell_measurement_reflns_used    1268
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.38
_cell_measurement_theta_min      2.29
_cell_volume                     2314.3(13)
_computing_cell_refinement       'Apex2 v2009.7-0'
_computing_data_collection       'Apex2 v2009.7-0 (Bruker, 2009)'
_computing_data_reduction        'Apex2 v2009.7-0'
_computing_molecular_graphics    'SHELXTL 6.14'
_computing_publication_material  'SHELXTL 6.14'
_computing_structure_refinement  'SHELXTL 6.14'
_computing_structure_solution
'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0880
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20289
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2009.7-0 (Bruker, 2009)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.379
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         8112
_refine_ls_number_restraints     327
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+1.7732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.2130
_reflns_number_gt                4433
_reflns_number_total             8112
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3ob40138c.txt
_cod_data_source_block           10mz486_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2314.3(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7152931