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_4066696
_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         'C14 O15 Ru5, 2(C7 H10 N)'
_chemical_formula_sum            'C28 H20 N2 O15 Ru5'
_chemical_formula_weight         1129.81
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 100.590(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3856(3)
_cell_length_b                   39.4723(14)
_cell_length_c                   9.4818(2)
_cell_measurement_reflns_used    3674
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.9884
_cell_measurement_theta_min      3.3466
_cell_volume                     3452.90(18)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.865
_diffrn_measured_fraction_theta_max 0.865
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_av_sigmaI/netI    0.1533
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11957
_diffrn_reflns_theta_full        70.12
_diffrn_reflns_theta_max         70.12
_diffrn_reflns_theta_min         4.48
_exptl_absorpt_coefficient_mu    17.949
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) 
(compiled Oct 18 2006,16:28:17) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.183
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [0.00000+1.00000exp(1.50(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0629P)^2^+0.0000sin\q/\l]
 where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                3035
_reflns_number_total             5699
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om100574j_si_002.cif
_cod_data_source_block           g182rosin
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4066696