Allenyl to Alkenylcarbyne Tautomerization at the Ru‒Si Bond of Ru(κP,P,Si) Pincer Complexes
Bernal, María J.; Martín, Marta; Sola, Eduardo; Organometallics 34 (2015) 800–; doi:10.1021/om501238d

data_4085458
_publ_section_title
;
 Allenyl to Alkenylcarbyne Tautomerization at the Ru--Si Bond of
 Ru(\kP,P,Si) Pincer Complexes
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              800
_journal_paper_doi               10.1021/om501238d
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C30 H46 Cl2 P2 Ru Si, 2(C H2 Cl2)'
_chemical_formula_sum            'C32 H50 Cl6 P2 Ru Si'
_chemical_formula_weight         838.52
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.3720(10)
_cell_angle_beta                 84.2390(10)
_cell_angle_gamma                68.6740(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8915(7)
_cell_length_b                   11.2760(8)
_cell_length_c                   18.3524(13)
_cell_measurement_reflns_used    8572
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      29.49
_cell_measurement_theta_min      2.24
_cell_volume                     1893.0(2)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.10,BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20015
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         1.12
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
  within SAINT+ package, v. 6.01.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.593
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         9611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                7839
_reflns_number_total             9611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501238d_si_001.cif
_cod_data_source_block           mo_mar203a
_cod_depositor_comments
'Adding full bibliography for 4085457--4085458.cif.'
_cod_database_code               4085458