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_4333857
_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         'C38 H32.50 Co0.75 N6, C38 H32.58 Co0.71 N6'
_chemical_formula_sum            'C76 H65.09 Co1.45 N12'
_chemical_formula_weight         1231.94
_chemical_name_systematic
; 
 ? 
;
_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                82.306(14)
_cell_angle_beta                 85.505(15)
_cell_angle_gamma                87.510(16)
_cell_formula_units_Z            1
_cell_length_a                   6.842(7)
_cell_length_b                   14.204(14)
_cell_length_c                   14.982(15)
_cell_measurement_reflns_used    1021
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      3.0
_cell_volume                     1438(2)
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_collection       'Apex2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2011)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  silicon(111)
_diffrn_radiation_source         'Beamline 11.3.1 ALS'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.179
_diffrn_reflns_av_sigmaI/netI    0.192
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16946
_diffrn_reflns_theta_full        25.44
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       needle
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.208
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         4068
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1989
_refine_ls_R_factor_gt           0.1135
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1462P)^2^+5.8197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2729
_refine_ls_wR_factor_ref         0.3211
_reflns_number_gt                2248
_reflns_number_total             4068
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic302150j_si_002_05.cif
_cod_data_source_block           CoL
_cod_database_code               4333857