Isolation of Ruthenium‒Indolizine Complexes: Insight into the Metal-Induced Cycloisomerization of Propargylic Pyridines
Chung, Lai-Hon; Wong, Chun-Yuen; Organometallics 32 (2013) 3583–; doi:10.1021/om400550w

data_4081175
_publ_section_title
;
 Isolation of Ruthenium--Indolizine Complexes: Insight into the
 Metal-Induced Cycloisomerization of Propargylic Pyridines
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3583
_journal_paper_doi               10.1021/om400550w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C31 H34 Cl2 N4 O11 Ru S3'
_chemical_formula_weight         906.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 111.925(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.8120(10)
_cell_length_b                   11.3346(4)
_cell_length_c                   27.0778(12)
_cell_measurement_reflns_used    8209
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.6035
_cell_measurement_theta_min      3.4428
_cell_volume                     7349.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            13358
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    6.938
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.35.21'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0350P)^2^+12.1657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0657
_reflns_number_gt                6324
_reflns_number_total             6577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400550w_si_002.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        7349.1(5)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4081175