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_4329101
_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         'C24 H40 Cl2 N12 Re2, F6 P, 2(C Cl2)'
_chemical_formula_sum            'C26 H40 Cl6 F6 N12 P Re2'
_chemical_formula_weight         1250.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n 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                   16.853(9)
_cell_length_b                   24.998(13)
_cell_length_c                   9.728(5)
_cell_measurement_reflns_used    6252
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      23.79
_cell_measurement_theta_min      2.24
_cell_volume                     4098(4)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SMART (Bruker, 2001)'
_computing_molecular_graphics    'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       'phi and 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  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            32940
_diffrn_reflns_theta_full        25.57
_diffrn_reflns_theta_max         25.57
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.397
_exptl_absorpt_correction_T_max  0.4470
_exptl_absorpt_correction_T_min  0.3610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_description       block
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.947
_refine_diff_density_min         -1.801
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3933
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0530P)^2^+26.8721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1378
_reflns_number_gt                2859
_reflns_number_total             3933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300169f_si_001_1.cif
_cod_data_source_block           Re2_(tbn)4_Cl2_PF6_(1)
_cod_database_code               4329101