Structural, Electrochemical, and Spectroscopic Investigation of Acetate Bridged Dinuclear Tetrakis-Schiff Base Macrocycles of Mn and Zn
Subhadeep Kal; Alexander S. Filatov; Peter H. Dinolfo; Inorganic Chemistry 52 (2013) 13963–13973; doi:10.1021/ic401631e

data_4336964
_publ_contact_author_address
;
Department of Chemistry & Chemical Biology
Rensselaer Polytechnic Institute
110 8th Street, 125 Cogswell Lab
Troy, NY 12180
USA
;
_publ_contact_author_email       dinolp@rpi.edu
_publ_contact_author_fax         518-276-4887
_publ_contact_author_name
;
Dinolfo, Peter H.
;
_publ_contact_author_phone       518-276-2326
_publ_section_title
;
 Structural, Electrochemical, and Spectroscopic Investigation of Acetate
 Bridged Dinuclear Tetrakis-Schiff Base Macrocycles of Mn and Zn
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13963
_journal_page_last               13973
_journal_paper_doi               10.1021/ic401631e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C36 H51 N6 O4 Zn2, F6 P'
_chemical_formula_sum            'C36 H51 F6 N6 O4 P Zn2'
_chemical_formula_weight         907.54
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 106.093(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.290(2)
_cell_length_b                   16.324(3)
_cell_length_c                   21.628(4)
_cell_measurement_reflns_used    8123
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.1344
_cell_measurement_theta_min      2.3235
_cell_volume                     4169.0(13)
_computing_cell_refinement       'SAINT Ver. 6.22  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '0.30\% \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35941
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_T_max  0.8433
_exptl_absorpt_correction_T_min  0.8238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
;
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         9811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0596P)^2^+2.4065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                7763
_reflns_number_total             9811
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic401631e_si_002_2.cif
_cod_data_source_block           '[Zn2LAc](PF6)'
_cod_original_cell_volume        4169.0(12)
_cod_original_sg_symbol_Hall     '-P 2ybc     '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4336964