Direct Evidence from Electron Paramagnetic Resonance for Additional Configurations in Uncommon Paddlewheel Re27+ Units Surrounded by an Unsymmetrical Bicyclic Guanidinate
Gina M. Chiarella; F. Albert Cotton; Naresh S. Dalal; Carlos A. Murillo; Zhenxing Wang; Mark D. Young; Inorganic Chemistry 51 (2012) 5257–5263; doi:10.1021/ic300169f

data_4329103
_publ_section_title
;
 Direct Evidence from Electron Paramagnetic Resonance for Additional
 Configurations in Uncommon Paddlewheel Re27+ Units Surrounded by an
 Unsymmetrical Bicyclic Guanidinate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5257
_journal_page_last               5263
_journal_paper_doi               10.1021/ic300169f
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C30 H46 F6 N12 O6 Re2 S2, 0.6(O6 S2),C4, 0.79(C F3), C2, 2(C)'
_chemical_formula_sum            'C38.75 H46 F8.5 N12 O9.5 Re2 S3.25'
_chemical_formula_weight         1469.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           67
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2'
_symmetry_space_group_name_H-M   'C m m a'
_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            4
_cell_length_a                   16.5175(13)
_cell_length_b                   17.4347(14)
_cell_length_c                   17.5012(14)
_cell_measurement_reflns_used    9673
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.33
_cell_volume                     5040.0(7)
_computing_cell_refinement       'APEX-II(BRUKER-NONIUS, 2008)'
_computing_data_collection       'APEX-II (BRUKER-NONIUS, 2008)'
_computing_data_reduction        'APEX-II (BRUKER-NONIUS, 2008'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Bruker 2000)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'APEX II'
_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  0.1072
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25681
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.031
_exptl_absorpt_correction_T_max  0.6331
_exptl_absorpt_correction_T_min  0.4328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_description       block
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.788
_refine_diff_density_min         -2.634
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2670
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0606P)^2^+156.6367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                2241
_reflns_number_total             2670
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300169f_si_001_3.cif
_cod_data_source_block           Re2_hpp_4_SO3CF3_3_(3)
_cod_original_formula_sum        'C38.75 H46 F8.50 N12 O9.50 Re2 S3.25'
_cod_database_code               4329103