Preparation, Structural Characterization, Assessment of Potential Antiaromaticity and Metalation of 21-Oxyazuliporphyrins.
Lash, Timothy D.; Colby, Denise A.; El-Beck, Jessica A; AbuSalim, Deyaa I.; Ferrence, Gregory M.; Inorganic chemistry 54 (2015) 9174–9187; doi:10.1021/acs.inorgchem.5b01587

data_4344103
_publ_section_title
;
 Preparation, Structural Characterization, Assessment of Potential
 Antiaromaticity and Metalation of 21-Oxyazuliporphyrins.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9174
_journal_page_last               9187
_journal_paper_doi               10.1021/acs.inorgchem.5b01587
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C50 H31 N3 O1 Pd1'
_chemical_formula_sum            'C50 H31 N3 O Pd'
_chemical_formula_weight         796.18
_chemical_name_systematic
;
(5,10,15,20-tetraphenyl-21-oxyazuliporphyrinato)-palladium(ii)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2014/7
_cell_angle_alpha                67.543(2)
_cell_angle_beta                 87.729(2)
_cell_angle_gamma                86.299(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3316(3)
_cell_length_b                   13.7733(4)
_cell_length_c                   14.5539(4)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.88
_cell_measurement_theta_min      2.59
_cell_volume                     1724.88(9)
_computing_cell_refinement       'APEX2 & SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and 
<i>Mercury CSD</i> (Macrae et al., 2008)
;
_computing_publication_material
;
<i>WinGX</i> (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-2014 (Burla, et. al, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker APEX-II CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            69743
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.351
_diffrn_reflns_theta_min         1.736
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.7124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2014.7-1 (Bruker, 2014)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         11584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0360P)^2^+2.0960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                9421
_reflns_number_total             11584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01587_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4344103--4344104.cif.'
_cod_original_formula_sum        'C50 H31 N3 O1 Pd1'
_cod_database_code               4344103
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.917
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              25003
_shelx_hkl_checksum              12654