Triple-Stranded Helicates of Zinc(II) and Cadmium(II) Involving a New Redox-Active Multiring Nitrogenous Heterocyclic Ligand: Synthesis, Structure, and Electrochemical and Photophysical Properties
Nabanita Kundu; Sk Md Towsif Abtab; Sanchita Kundu; Akira Endo; Simon J. Teat; Muktimoy Chaudhury; Inorganic Chemistry 51 (2012) 2652–2661; doi:10.1021/ic202595p

data_4328445
_publ_section_title
;
 Triple-Stranded Helicates of Zinc(II) and Cadmium(II) Involving a New
 Redox-Active Multiring Nitrogenous Heterocyclic Ligand: Synthesis,
 Structure, and Electrochemical and Photophysical Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2652
_journal_page_last               2661
_journal_paper_doi               10.1021/ic202595p
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C72 H51 Cd2 Cl4 N18 O17.5'
_chemical_formula_weight         1814.91
_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                91.733(2)
_cell_angle_beta                 96.585(3)
_cell_angle_gamma                106.162(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9650(15)
_cell_length_b                   15.101(2)
_cell_length_c                   22.596(3)
_cell_measurement_reflns_used    7140
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      2.23
_cell_volume                     3562.3(8)
_computing_cell_refinement       'Bruker SAINT v7.23a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v7.23a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Platinum 200 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0730
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26166
_diffrn_reflns_theta_full        25.63
_diffrn_reflns_theta_max         25.63
_diffrn_reflns_theta_min         1.53
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2004/1 Bruker AXS Madison WI, US'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       needle
_exptl_crystal_F_000             1826
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.667
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         10350
_refine_ls_number_restraints     1096
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0729
_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^)+(0.1040P)^2^+8.2966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.2011
_reflns_number_gt                7312
_reflns_number_total             10350
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic202595p_si_002_3.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C72 H51 Cd2 Cl4 N18 O17.50'
_cod_database_code               4328445