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_4114095
_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
'(C128H128N16O36Cl4Ru8) (C2H3N) (C6H14)2 (H2O)12'
_chemical_formula_sum            'C142 H183 Cl4 N17 O48 Ru8'
_chemical_formula_weight         3846.41
_chemical_name_common
'{cis-(DAniF)2Ru2Cl(oxalate)(H2O)}4 (CH3CN) 2(C6H14) 12H2O'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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            2
_cell_length_a                   19.9157(14)
_cell_length_b                   19.9157(14)
_cell_length_c                   25.760(4)
_cell_measurement_reflns_used    8338
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      2.42
_cell_volume                     10217.3(19)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        'SAINT and SADABS'
_computing_molecular_graphics    'SHELXTL V6.10 (Bruker, 2000)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       'w/ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19332
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  0.8566
_exptl_absorpt_correction_T_min  0.7424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V1.03'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             3916
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3426
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0820
_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^)+(0.0820P)^2^+267.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1973
_refine_ls_wR_factor_ref         0.2443
_reflns_number_gt                2353
_reflns_number_total             3426
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036095xsi20030512_050600_3.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        10217.1(18)
_cod_database_code               4114095