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_4331042
_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         'C20 H40 K O8, C28 H30 Mn N2'
_chemical_formula_sum            'C48 H70 K Mn N2 O8'
_chemical_formula_weight         897.10
_chemical_name_systematic
; 
[K(18-crown-6)(THF)2][Mn(2,2'bipy)(C9H11)2]
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.0840(2)
_cell_length_b                   32.1910(4)
_cell_length_c                   23.1510(3)
_cell_measurement_reflns_used    4379
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.4064
_cell_measurement_theta_min      2.5276
_cell_volume                     9750.9(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_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  'Rigaku KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Double Si-111 crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10294
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.9919
_exptl_absorpt_correction_T_min  0.9527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       plate
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4039
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+3.5375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                3540
_reflns_number_total             4039
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic301587f_si_002_5.cif
_cod_data_source_block           2-(a)
_cod_original_sg_symbol_Hall     'P 2c -2n'
_cod_database_code               4331042