Trapping of Pyrid-2-ylidenes by [Ru3(CO)12]: Orthometalated Pyrid-2-ylidenes in Triruthenium Clusters
Cabeza, Javier A.; del Río, Ignacio; Pérez-Carreño, Enrique; Sánchez-Vega, M. Gabriela; Vázquez-García, Digna; Organometallics 29 (2010) 4464–; doi:10.1021/om100574j

data_4066694
_publ_section_title
;
 Trapping of Pyrid-2-ylidenes by [Ru3(CO)12]: Orthometalated
 Pyrid-2-ylidenes in Triruthenium Clusters
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4464
_journal_paper_doi               10.1021/om100574j
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C16 H9 N O9 Ru3, 0.25(C6)'
_chemical_formula_sum            'C17.5 H9 N O9 Ru3'
_chemical_formula_weight         680.46
_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                80.4720(10)
_cell_angle_beta                 71.7850(10)
_cell_angle_gamma                79.7350(10)
_cell_formula_units_Z            2
_cell_length_a                   9.630(2)
_cell_length_b                   9.910(2)
_cell_length_c                   12.358(3)
_cell_measurement_reflns_used    3396
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      1.018
_cell_volume                     1094.7(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_molecular_graphics    'PLATON (Spek, 2006)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10691
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    2.090
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.095
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.297
_refine_ls_extinction_coef       0.000(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         3640
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [1.00000+-1.00000exp(-20.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+2.6015*P+(0.1343P)^2^+0.0000sin\q/\l]
 where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1695
_refine_ls_wR_factor_ref         0.1996
_reflns_number_gt                2783
_reflns_number_total             3640
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100574j_si_002.cif
_cod_data_source_block           g182f2k
_cod_database_code               4066694