On the Structural and Electronic Properties of [Zn2(4,4'-bipyridine)(mes)4]n- (n= 0-2), a Homologous Series of Bimetallic Complexes Bridged by Neutral, Anionic, and Dianionic 4,4'-Bipyridine
Mark Irwin; Tobias Krämer; John E. McGrady; Jose M. Goicoechea; Inorganic Chemistry 50 (2011) 5006–5014; doi:10.1021/ic200241d

data_4325203
_publ_contact_author
;
 Dr. J. M. Goicoechea           
 Chemistry Research Laboratory
 University of Oxford
 Mansfield Road
 Oxford
 OX1 3TA
 UK
;
_publ_contact_author_email       jose.goicoechea@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 272690'
_publ_contact_author_phone       '+44 1865 275961'
_publ_section_title
;
 On the Structural and Electronic Properties of
 [Zn2(4,4'-bipyridine)(mes)4]n- (n= 0-2), a Homologous Series of
 Bimetallic Complexes Bridged by Neutral, Anionic, and Dianionic
 4,4'-Bipyridine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5006
_journal_page_last               5014
_journal_paper_doi               10.1021/ic200241d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C46 H52 N2 Zn2, C20 H40 K O8'
_chemical_formula_sum            'C66 H92 K N2 O8 Zn2'
_chemical_formula_weight         1211.26
_chemical_name_systematic
; 
[K(18-crown-6)THF2][Zn2(4,4'-bipy)(Mes)4]
;
_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                76.111(1)
_cell_angle_beta                 81.897(1)
_cell_angle_gamma                61.729(1)
_cell_formula_units_Z            6
_cell_length_a                   20.6965(1)
_cell_length_b                   20.8215(1)
_cell_length_c                   27.0298(1)
_cell_measurement_reflns_used    45066
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     9953.61(13)
_computing_cell_refinement
;
KappaCCD software "DENZO" (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
KappaCCD software "Collect" (Nonius, 2000)
;
_computing_data_reduction
;
KappaCCD software "DENZO" (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            89021
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         5.10
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.8244
_exptl_absorpt_correction_T_min  0.7755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       block
_exptl_crystal_F_000             3870
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.441
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2134
_refine_ls_number_reflns         45306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+6.4038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1309
_reflns_number_gt                33744
_reflns_number_total             45306
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic200241d_si_002_3.cif
_cod_data_source_block           2b
_cod_original_cell_volume        9953.6(1)
_cod_database_code               4325203