Chiral Cationic Cp(x)Ru(II) Complexes for Enantioselective Yne-Enone Cyclizations.
Kossler, David; Cramer, Nicolai; Journal of the American Chemical Society 137 (2015) 12478–12481; doi:10.1021/jacs.5b08232

data_4124735
_publ_section_title
;
 Chiral Cationic Cp(x)Ru(II) Complexes for Enantioselective Yne-Enone
 Cyclizations.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12478
_journal_page_last               12481
_journal_paper_doi               10.1021/jacs.5b08232
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C35 H29 O2 Ru, F6 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C37 H33 Cl4 F6 O2 P Ru'
_chemical_formula_weight         897.47
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-15 # Formatted by publCIF

;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.195(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7297(3)
_cell_length_b                   17.7981(5)
_cell_length_c                   11.6078(4)
_cell_measurement_reflns_used    8478
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      72.9580
_cell_measurement_theta_min      4.5350
_cell_volume                     1780.35(10)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 10.2665
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11980
_diffrn_reflns_theta_full        73.30
_diffrn_reflns_theta_max         73.30
_diffrn_reflns_theta_min         3.86
_exptl_absorpt_coefficient_mu    7.334
_exptl_absorpt_correction_T_max  0.342
_exptl_absorpt_correction_T_min  0.220
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.690
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(13)
_refine_ls_extinction_coef       0.0021(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5095
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+2.1703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                4966
_reflns_number_total             5095
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b08232_si_002.cif
_cod_data_source_block           dko-1-291
_cod_original_cell_volume        1780.35(11)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4124735
_publcif_datablock.id            {6247e198-c5e8-42e0-bf12-7e8be8663615}
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n