Group 6 Complexes with Iron and Zinc Heterometals: Understanding the Structural, Spectroscopic, and Electrochemical Properties of a Complete Series of M M...M' Compounds
Michael Nippe; Eckhard Bill; John F. Berry; Inorganic Chemistry 50 (2011) 7650–7661; doi:10.1021/ic2011315

data_4325965
_publ_contact_author_address
;Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI  53706
USA
;
_publ_contact_author_email       berry@chem.wisc.edu
_publ_contact_author_name        'John F. Berry'
_publ_contact_author_phone       809-608-262-7534
_publ_section_title
;
 Group 6 Complexes with Iron and Zinc Heterometals: Understanding the
 Structural, Spectroscopic, and Electrochemical Properties of a Complete
 Series of M M...M' Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7650
_journal_page_last               7661
_journal_paper_doi               10.1021/ic2011315
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C40 H32 N12 Cr2 Zn2 Cl4, 1.5 (C4H8O), C4H10'
_chemical_formula_sum            'C48 H50 Cl4 Cr2 N12 O2 Zn2'
_chemical_formula_weight         1203.54
_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                62.5790(10)
_cell_angle_beta                 70.665(2)
_cell_angle_gamma                78.582(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6107(4)
_cell_length_b                   15.2039(5)
_cell_length_c                   16.3625(5)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.9917
_cell_measurement_theta_min      2.3460
_cell_volume                     2623.80(15)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL, OLEX2 (Dolomanov et al., 2009)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            65867
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    1.561
_exptl_absorpt_correction_T_max  0.8814
_exptl_absorpt_correction_T_min  0.7322
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       needle
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         1.848
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         12682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+4.3043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                11294
_reflns_number_total             12682
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2011315_si_002_6.cif
_cod_data_source_block           berry166c
_cod_original_cell_volume        2623.80(14)
_cod_database_code               4325965