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_4328678
_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_formula_moiety         'C30 H22 Cr N6, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C34 H28 Cr F12 N8 P2'
_chemical_formula_weight         890.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_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                   12.3886(14)
_cell_length_b                   12.3886(14)
_cell_length_c                   48.243(6)
_cell_measurement_reflns_used    54498
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.9998
_cell_measurement_theta_min      2.6364
_cell_volume                     7404.2(15)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-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  0.0675
_diffrn_reflns_av_sigmaI/netI    0.0958
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            40737
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.98939
_exptl_absorpt_correction_T_min  0.96317
_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       platelet
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1089
_refine_ls_number_reflns         16282
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0147P)^2^+8.8953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                11735
_reflns_number_total             16282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2027219_si_002_1.cif
_cod_data_source_block           2
_cod_database_code               4328678