Structural investigation of 5,10-<i>A</i>~2~<i>B</i>~2~-type porphyrins: palladium(II) and zinc(II) complexes of 5,10-dibromo-15,20-bis(4-methylphenyl)porphyrin
Senge, Mathias O.; Zawadzka, Monika; Acta Crystallographica Section C 70 (2014) –; doi:10.1107/S2053229614023687

data_2019734
_publ_section_title
;
 Structural investigation of 5,10-<i>A</i>~2~<i>B</i>~2~-type porphyrins:
 palladium(II) and zinc(II) complexes of
 5,10-dibromo-15,20-bis(4-methylphenyl)porphyrin
;
_journal_coeditor_code           OV3055
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614023687
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Pd (C34 H22 Br2 N4)]'
_chemical_formula_moiety         'C34 H22 Br2 N4 Pd'
_chemical_formula_sum            'C34 H22 Br2 N4 Pd'
_chemical_formula_weight         752.78
_chemical_name_systematic
;
[5,10-Dibromo-15,20-bis(4-methylphenyl)porphyrinato]palladium(II)
;
_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                95.157(8)
_cell_angle_beta                 103.433(8)
_cell_angle_gamma                107.007(8)
_cell_formula_units_Z            2
_cell_length_a                   9.396(4)
_cell_length_b                   10.558(5)
_cell_length_c                   15.129(7)
_cell_measurement_reflns_used    871
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.36
_cell_volume                     1375.7(11)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2005)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2005)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2005)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10757
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.612
_exptl_absorpt_correction_T_max  0.7861
_exptl_absorpt_correction_T_min  0.3646
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2005)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.501
_refine_diff_density_min         -1.360
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         4833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1228P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1802
_reflns_number_gt                3628
_reflns_number_total             4833
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ov3055sup1.cif
_cod_data_source_block           V
_cod_original_cell_volume        1375.7(10)
_cod_database_code               2019734
_cod_database_fobs_code          2019734