A Homologous Series of First-Row Transition-Metal Complexes of 2,2'-Bipyridine and their Ligand Radical Derivatives: Trends in Structure, Magnetism, and Bonding
Mark Irwin; Laurence R. Doyle; Tobias Krämer; Radovan Herchel; John E. McGrady; Jose M. Goicoechea; Inorganic Chemistry 51 (2012) 12301–12312; doi:10.1021/ic301587f

data_4331041
_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
;
 A Homologous Series of First-Row Transition-Metal Complexes of
 2,2'-Bipyridine and their Ligand Radical Derivatives: Trends in
 Structure, Magnetism, and Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12301
_journal_page_last               12312
_journal_paper_doi               10.1021/ic301587f
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C28 H30 Cr N2, C24 H32 K O7, 2(C4 H8 O)'
_chemical_formula_sum            'C60 H78 Cr K N2 O9'
_chemical_formula_weight         1062.34
_chemical_name_systematic
; 
[K(dibenzo-18-crown-6)THF][Cr(2,2'-bipy)(Mes)2]*2THF
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 107.5610(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2207(2)
_cell_length_b                   13.7416(2)
_cell_length_c                   29.9804(5)
_cell_measurement_reflns_used    83176
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      5.097
_cell_volume                     5585.59(15)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            18045
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         5.13
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  0.9834
_exptl_absorpt_correction_T_min  0.8497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       plate
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         9745
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+2.9633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                6655
_reflns_number_total             9745
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic301587f_si_002_4.cif
_cod_data_source_block           1-
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_database_code               4331041