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_4114096
_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
'(C200.72H206.38N21.414O32Cl2.586Ru8)+, (Cl1.414)-, (C2H4Cl2)17, (C6H14)'
_chemical_formula_sum            'C240.72 H288.38 Cl38 N21.41 O32 Ru8'
_chemical_formula_weight         6149.40
_chemical_name_systematic
; 
 ? 
;
_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                89.698(1)
_cell_angle_beta                 66.277(1)
_cell_angle_gamma                70.313(1)
_cell_formula_units_Z            1
_cell_length_a                   19.2080(11)
_cell_length_b                   20.6163(12)
_cell_length_c                   22.5781(13)
_cell_measurement_reflns_used    7418
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.21
_cell_volume                     7618.4(8)
_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      193(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42383
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.81
_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    0.778
_exptl_absorpt_correction_T_max  0.8174
_exptl_absorpt_correction_T_min  0.7246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V1.03'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             3137
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.463
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1704
_refine_ls_number_reflns         25735
_refine_ls_number_restraints     1761
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0663P)^2^+39.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1724
_refine_ls_wR_factor_ref         0.1926
_reflns_number_gt                17862
_reflns_number_total             25735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja036095xsi20030512_050600_4.cif
_cod_data_source_block           compound3
_cod_database_code               4114096