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_4075684
_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_compound_source
;
Synthesis. Crystallization from a CH~2~Cl~2~ /
 hexanes solution 
at room temperature by slow liquid-liquid difussion.
;
_chemical_formula_moiety         'C26 H18 N2 O8 Ru3, 0.5(C6 H14)'
_chemical_formula_sum            'C29 H25 N2 O8 Ru3'
_chemical_formula_weight         832.72
_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                78.326(2)
_cell_angle_beta                 89.038(2)
_cell_angle_gamma                78.554(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5945(3)
_cell_length_b                   12.3050(3)
_cell_length_c                   13.4399(4)
_cell_measurement_temperature    120(2)
_cell_volume                     1522.54(8)
_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      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.065
_diffrn_reflns_av_sigmaI/netI    0.1038
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30385
_diffrn_reflns_theta_full        68.41
_diffrn_reflns_theta_max         68.41
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    12.335
_exptl_absorpt_correction_T_max  0.216
_exptl_absorpt_correction_T_min  0.087
_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    1.816
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             818
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.125
_refine_diff_density_max         1.690
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.202
_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     379
_refine_ls_number_reflns         5563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1378
_reflns_number_gt                5083
_reflns_number_total             5563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049119xsi20041203_123105.cif
_cod_data_source_block           3b_(lm32f3)
_cod_database_code               4075684