Synthesis, Structural Characterization, Aromatic Characteristics, and Metalation of Neo-Confused Porphyrins, a Newly Discovered Class of Porphyrin Isomers.
Li, Ruoshi; Lammer, Aaron D.; Ferrence, Gregory M.; Lash, Timothy D.; The Journal of organic chemistry 79 (2014) 4078–4093; doi:10.1021/jo500580e

data_4029319
_publ_section_title
;
 Synthesis, Structural Characterization, Aromatic Characteristics, and
 Metalation of Neo-Confused Porphyrins, a Newly Discovered Class of
 Porphyrin Isomers.
;
_journal_issue                   9
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              4078
_journal_page_last               4093
_journal_paper_doi               10.1021/jo500580e
_journal_volume                  79
_journal_year                    2014
_chemical_formula_moiety         'C30 H30 N4 O2 Pd1'
_chemical_formula_sum            'C30 H30 N4 O2 Pd'
_chemical_formula_weight         584.98
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-01-03T12:23:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                105.580(4)
_cell_angle_beta                 91.632(4)
_cell_angle_gamma                97.148(4)
_cell_formula_units_Z            2
_cell_length_a                   8.1266(4)
_cell_length_b                   10.9322(6)
_cell_length_c                   14.5533(8)
_cell_measurement_reflns_used    7223
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.124
_cell_measurement_theta_min      2.531
_cell_volume                     1233.16(12)
_computing_cell_refinement       'APEX2 & SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
<i>Ortep-3</i> for Windows (Farrugia, 2012) and <i>Mercury CSD</i> (Macrae et
 al., 2008)
;
_computing_publication_material
;
        <i>WinGX</i> (Farrugia, 2012) and <i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_details
;
3672 frames were collected.  The total exposure time was 15.30 hours.
;
_diffrn_measurement_device_type  'Bruker APEX-II CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1059
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47424
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.998
_diffrn_reflns_theta_min         1.952
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2013.2-0 (Bruker, 2013)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.628
_refine_diff_density_min         -2.245
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         8107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.6258P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                5968
_reflns_number_total             8107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo500580e_si_006.cif
_cod_data_source_block           gmf13024
_cod_depositor_comments
'Adding full bibliography for 4029318--4029321.cif.'
_cod_database_code               4029319