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_4329102
_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, 6(C H Cl3), Cl '
_chemical_formula_sum            'C30 H46 Cl21 N12 Re2'
_chemical_formula_weight         1691.64
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.469(12)
_cell_angle_beta                 79.659(12)
_cell_angle_gamma                79.016(12)
_cell_formula_units_Z            1
_cell_length_a                   10.046(8)
_cell_length_b                   10.935(8)
_cell_length_c                   13.492(10)
_cell_measurement_reflns_used    5536
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.09
_cell_volume                     1429.8(19)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9765
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.249
_exptl_absorpt_correction_T_max  0.4517
_exptl_absorpt_correction_T_min  0.4200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_description       block
_exptl_crystal_F_000             817
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.455
_refine_diff_density_min         -2.561
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4964
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0565P)^2^+4.4690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1316
_reflns_number_gt                3977
_reflns_number_total             4964
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300169f_si_001_2.cif
_cod_data_source_block           Re2_(tbn)4_Cl3_(2)
_cod_database_code               4329102