Mono- and Bisquinoline-Annulated Porphyrins from Porphyrin β,β'-Dione Oximes.
Akhigbe, Joshua; Luciano, Michael; Zeller, Matthias; Brückner, Christian; The Journal of organic chemistry 80 (2014) 499–; doi:10.1021/jo502511j

data_4030370
_publ_section_title
;
 Mono- and Bisquinoline-Annulated Porphyrins from Porphyrin \b,\b'-Dione
 Oximes.
;
_journal_issue                   1
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              499
_journal_paper_doi               10.1021/jo502511j
_journal_volume                  80
_journal_year                    2014
_chemical_formula_moiety         'C44 H24 N6 Pd, 0.3(C6 H14), 0.34(C H2 Cl2)'
_chemical_formula_sum            'C46.13 H28.86 Cl0.68 N6 Pd'
_chemical_formula_weight         797.52
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.9060(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6776(5)
_cell_length_b                   7.0794(2)
_cell_length_c                   32.3824(11)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.9367
_cell_measurement_theta_min      3.0124
_cell_volume                     3362.95(19)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2014)'
_computing_data_collection       'Apex2 v2014.1-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker, 2014)'
_computing_structure_refinement
;  
SHELXL-2013 (Sheldrick, 2013), 
SHELXLE Rev645 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker AXS Prospector CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            15657
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.070
_diffrn_reflns_theta_min         2.730
_diffrn_source                   'I-mu-S microsource X-ray tube'
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_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.6249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2014.1-0 (Bruker, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       rod
_exptl_crystal_F_000             1620.5
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         5917
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+7.0357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5604
_reflns_number_total             5917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo502511j_si_002.cif
_cod_data_source_block           Prosp14mz008_0m
_cod_depositor_comments
'Adding full bibliography for 4030367--4030370.cif.'
_cod_database_code               4030370
_shelx_estimated_absorpt_t_min   0.466
_shelx_estimated_absorpt_t_max   0.777
_shelxl_version_number           2013-4