Mechanism Investigations of the Endo Cycloisomerization of Alkynols through Isolation and Characterization of Ruthenium Complexes from the Reactions of Alkynes with a Ruthenium Complex
Liu, Pei Nian; Wen, Ting Bin; Ju, Kun Dong; Sung, Herman H.-Y.; Williams, Ian D.; Jia, Guochen; Organometallics 30 (2011) 2571–; doi:10.1021/om2001684

data_4064551
_publ_section_title
;
 Mechanism Investigations of the Endo Cycloisomerization of Alkynols
 through Isolation and Characterization of Ruthenium Complexes from the
 Reactions of Alkynes with a Ruthenium Complex
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2571
_journal_paper_doi               10.1021/om2001684
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C63.5 H64.5 B Cl2 N3 O P Ru'
_chemical_formula_weight         1099.43
_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                 93.945(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.8739(9)
_cell_length_b                   12.3263(4)
_cell_length_c                   27.7974(6)
_cell_measurement_reflns_used    5487
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.35
_cell_measurement_theta_min      4.24
_cell_volume                     11579.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.951
_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  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0895
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            16943
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         4.92
_exptl_absorpt_coefficient_mu    3.626
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4580
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.458
_refine_diff_density_min         -1.556
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         9833
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0548
_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 
 [0.00000+1.00000exp(0.80(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0700P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1329
_reflns_number_gt                6555
_reflns_number_total             9833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2001684_si_001.cif
_cod_data_source_block           Complex13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C63.50 H64.50 B Cl2 N3 O P Ru'
_cod_database_code               4064551