Indolenine meso-Substituted Dibenzotetraaza[14]annulene and Its Coordination Chemistry toward the Transition Metal Ions MnIII, FeIII, CoII, NiII, CuII, and PdII
Hamid Khaledi; Marilyn M. Olmstead; Hapipah Mohd Ali; Noel F. Thomas; Inorganic Chemistry 52 (2013) 1926–1941; doi:10.1021/ic302150j

data_4333862
_publ_section_title
;
 Indolenine meso-Substituted Dibenzotetraaza[14]annulene and Its
 Coordination Chemistry toward the Transition Metal Ions MnIII, FeIII,
 CoII, NiII, CuII, and PdII
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1926
_journal_page_last               1941
_journal_paper_doi               10.1021/ic302150j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C84 H80 N12 O8 Pd2'
_chemical_formula_sum            'C84 H80 N12 O8 Pd2'
_chemical_formula_weight         1598.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.367(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9154(3)
_cell_length_b                   32.9705(6)
_cell_length_c                   9.9792(2)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    87(2)
_cell_measurement_theta_max      57.78
_cell_measurement_theta_min      3.55
_cell_volume                     4097.49(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      87(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            37260
_diffrn_reflns_theta_full        56.92
_diffrn_reflns_theta_max         56.92
_diffrn_reflns_theta_min         3.79
_exptl_absorpt_coefficient_mu    4.027
_exptl_absorpt_correction_T_max  0.9238
_exptl_absorpt_correction_T_min  0.5651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2006)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       needle
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.680
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.272
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         5491
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+22.0007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1415
_reflns_number_gt                5086
_reflns_number_total             5491
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic302150j_si_002_10.cif
_cod_data_source_block           Pd2L2H4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4333862