Intramolecular cyclization of a diruthenium complex: insight into the mechanism of heteroatom-directed intramolecular C-H/olefin coupling reactions.
Gong, Dawei; Hu, Bowen; Shi, Jing; Chen, Dafa; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12507–12510; doi:10.1039/c5dt02071a

data_7035384
_publ_section_title
;
 Intramolecular cyclization of a diruthenium complex: insight into the
 mechanism of heteroatom-directed intramolecular C-H/olefin coupling
 reactions.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12507
_journal_page_last               12510
_journal_paper_doi               10.1039/c5dt02071a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C24 H17 N O4 Ru2'
_chemical_formula_weight         585.53
_chemical_name_systematic
{(C5H4N)(?2-\h3,\h5-C9H5CCH2CH2CH2CCH2)}Ru2(CO)4
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-07 deposited with the CCDC.
2015-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 120.579(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.155(5)
_cell_length_b                   9.626(3)
_cell_length_c                   31.755(7)
_cell_measurement_temperature    296(2)
_cell_volume                     4251(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            14062
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.452
_exptl_absorpt_correction_T_max  0.7406
_exptl_absorpt_correction_T_min  0.7040
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/hexane'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         4026
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+7.2491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                3359
_reflns_number_total             4026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02071a2.cif
_cod_data_source_block           gaw021
_cod_depositor_comments
'Adding full bibliography for 7035384--7035385.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7035384