Experimental Fingerprints for Redox-Active Terpyridine in [Cr(tpy)2](PF6)n (n = 3-0), and the Remarkable Electronic Structure of [Cr(tpy)2]1-
Christopher C. Scarborough; Kyle M. Lancaster; Serena DeBeer; Thomas Weyhermüller; Stephen Sproules; Karl Wieghardt; Inorganic Chemistry 51 (2012) 3718–3732; doi:10.1021/ic2027219

data_4328681
_publ_section_title
;
 Experimental Fingerprints for Redox-Active Terpyridine in
 [Cr(tpy)2](PF6)n (n = 3-0), and the Remarkable Electronic Structure of
 [Cr(tpy)2]1-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3718
_journal_page_last               3732
_journal_paper_doi               10.1021/ic2027219
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        Pentadecane
_chemical_formula_moiety         'C30 H22 Mo N6'
_chemical_formula_sum            'C30 H22 Mo N6'
_chemical_formula_weight         562.48
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_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_block_code                7335
_audit_creation_date             2011-04-11
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            32
_cell_length_a                   39.484(6)
_cell_length_b                   56.962(8)
_cell_length_c                   8.3177(12)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.4835
_cell_measurement_theta_min      2.1830
_cell_volume                     18707(5)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0915
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       86
_diffrn_reflns_limit_k_min       -86
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            149541
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  0.99101
_exptl_absorpt_correction_T_min  0.69481
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       needle
_exptl_crystal_F_000             9152
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.095(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         16940
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0210P)^2^+32.8804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0659
_reflns_number_gt                14174
_reflns_number_total             16940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2027219_si_002_4.cif
_cod_data_source_block           5
_cod_database_code               4328681