Syntheses and Electronic Structure of Bimetallic Complexes Containing a Flexible Redox-Active Bridging Ligand
Stacey Lindsay; Siu K. Lo; Oliver R. Maguire; Eckhard Bill; Michael R. Probert; Stephen Sproules; Corinna R. Hess; Inorganic Chemistry 52 (2013) 898–909; doi:10.1021/ic302087f

data_4333589
_publ_section_title
;
 Syntheses and Electronic Structure of Bimetallic Complexes Containing a
 Flexible Redox-Active Bridging Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              898
_journal_page_last               909
_journal_paper_doi               10.1021/ic302087f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C24 H21 Cl4 N5 Zn2'
_chemical_formula_sum            'C24 H21 Cl4 N5 Zn2'
_chemical_formula_weight         652.00
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                77.8560(10)
_cell_angle_beta                 87.9490(10)
_cell_angle_gamma                72.3700(10)
_cell_formula_units_Z            2
_cell_length_a                   7.1827(2)
_cell_length_b                   9.4410(2)
_cell_length_c                   20.2740(4)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.33
_cell_measurement_theta_min      2.23
_cell_volume                     1280.35(5)
_computing_cell_refinement       'SAINT v8.18C (Bruker, 2012)'
_computing_data_collection       'Proteum2 (Bruker, 2010)'
_computing_data_reduction        'SAINT v8.18C (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker Pt 135 CCD area detector'
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Pt 135 CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focused optics'
_diffrn_radiation_monochromator  'Bruker Helios multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54188
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18576
_diffrn_reflns_theta_full        68.54
_diffrn_reflns_theta_max         68.54
_diffrn_reflns_theta_min         2.23
_diffrn_source                   'Microstar rotating anode'
_diffrn_source_target            Cu
_diffrn_source_type              'rotating anode'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.338
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1021 before and 0.0514 after correction.
The Ratio of minimum to maximum transmission is 0.6326.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       needle
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0241
_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^)+(0.0300P)^2^+1.1214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0645
_reflns_number_gt                4059
_reflns_number_total             4179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302087f_si_002_2.cif
_cod_data_source_block           compound_1
_cod_database_code               4333589
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H22 of C22, H4 of C4, {H13A,H13B} of C13, H24 of C24, H15 of C15, H6 of C6,
  H10 of C10, H18 of C18, {H19A,H19B} of C19, H21 of C21, H1 of C1, H17 of C17,
  H3 of C3, H8 of C8, H12 of C12, H2 of C2, H16 of C16, H23 of C23, H9 of C9
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C18(H18), C8(H8), C10(H10), C12(H12), C6(H6), C9(H9), C15(H15),
 C3(H3), C22(H22), C21(H21), C17(H17), C1(H1), C23(H23), C16(H16), C2(H2),
 C24(H24)
;