Molecular Squares with Paramagnetic Diruthenium Corners: Synthetic and Crystallographic Challenges
Panagiotis Angaridis; John F. Berry; F. Albert Cotton; Carlos A. Murillo; Xiaoping Wang; Journal of the American Chemical Society 125 (2003) 10327–10334; doi:10.1021/ja036095x

data_4114093
_publ_contact_author_address
;  Laboratory for Molecular Structure and Bonding
   Dept. of Chemistry
   Texas A&M University, P.O. Box  30012
   College Station, TX 77842-3012, USA
;
_publ_contact_author_email       cotton@tamu.edu
_publ_contact_author_fax         '(979) 845 9351'
_publ_contact_author_name        'F. A. Cotton'
_publ_contact_author_phone       '(979) 845 4432'
_publ_section_title
;
 Molecular Squares with Paramagnetic Diruthenium Corners: Synthetic and
 Crystallographic Challenges
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10327
_journal_page_last               10334
_journal_paper_doi               10.1021/ja036095x
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C42 H45 Cl2 N6 O4 Ru2, C2 H4 Cl4'
_chemical_formula_sum            'C44 H49 Cl5 N6 O4 Ru2'
_chemical_formula_weight         1105.28
_chemical_name_systematic
; 
cis-{[bis(mu-acetato)]-bis[(mu-di(p-tolyl)formamidinato)]diruthenium(II,III) 
chloride(p-tolylformamidine) dichloromethane solvate 
;
_space_group_IT_number           1
_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                69.1770(10)
_cell_angle_beta                 89.9160(10)
_cell_angle_gamma                74.7870(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0476(5)
_cell_length_b                   15.2900(8)
_cell_length_c                   17.8404(9)
_cell_measurement_reflns_used    7258
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.21
_cell_volume                     2459.1(2)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean '8.33 mm-1'
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker SMART 1000'
_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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15625
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.11
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.7804
_exptl_absorpt_correction_T_min  0.6792
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.560
_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   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1154
_refine_ls_number_reflns         12926
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                11178
_reflns_number_total             12926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036095xsi20030512_050600_1.cif
_cod_data_source_block           compound
_cod_database_code               4114093