η2-Edge-Bridging and η3-Face-Capping Coordination of Conjugated Ynenyl Ligands in Triruthenium Carbonyl Cluster Complexes Derived from 1,1-Dimethylhydrazine
Cabeza, Javier A.; del Río, Ignacio; García-Granda, Santiago; Martínez-Méndez, Lorena; Pérez-Carreño, Enrique; Organometallics 24 (2005) 831–; doi:10.1021/om049119x

data_4075683
_publ_section_title
;
 \h2-Edge-Bridging and \h3-Face-Capping Coordination of Conjugated Ynenyl
 Ligands in Triruthenium Carbonyl Cluster Complexes Derived from
 1,1-Dimethylhydrazine
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              831
_journal_paper_doi               10.1021/om049119x
_journal_volume                  24
_journal_year                    2005
_chemical_absolute_configuration ad
_chemical_compound_source
;
Synthesis. Crystallization from a CH~2~Cl~2~ /
 hexanes solution 
at room temperature by slow liquid-liquid difussion.
;
_chemical_formula_moiety         'C16 H14 N2 O8 Ru3'
_chemical_formula_sum            'C16 H14 N2 O8 Ru3'
_chemical_formula_weight         665.50
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   9.5729(3)
_cell_length_b                   13.1585(5)
_cell_length_c                   17.0702(6)
_cell_measurement_temperature    293(2)
_cell_volume                     2150.25(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'EUCLID (Spek, 1982)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_av_sigmaI/netI    0.0862
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44222
_diffrn_reflns_theta_full        68.44
_diffrn_reflns_theta_max         68.44
_diffrn_reflns_theta_min         4.24
_exptl_absorpt_coefficient_mu    17.249
_exptl_absorpt_correction_T_max  0.275
_exptl_absorpt_correction_T_min  0.156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.326
_refine_diff_density_min         -1.512
_refine_diff_density_rms         0.189
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3956
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0208P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                3159
_reflns_number_total             3956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049119xsi20041203_123105.cif
_cod_data_source_block           2a_(lm97f1)
_cod_database_code               4075683