Investigations into Ruthenium Metathesis Catalysts with Six-Membered Chelating NHC Ligands: Relationship between Catalyst Structure and Stereoselectivity
Endo, Koji; Herbert, Myles B.; Grubbs, Robert H.; Organometallics 32 (2013) 5128–; doi:10.1021/om4006966

data_4081414
_publ_section_title
;
 Investigations into Ruthenium Metathesis Catalysts with Six-Membered
 Chelating NHC Ligands: Relationship between Catalyst Structure and
 Stereoselectivity
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5128
_journal_paper_doi               10.1021/om4006966
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C41 H48 N2 O3 Ru, C H2 Cl2'
_chemical_formula_sum            'C42 H50 Cl2 N2 O3 Ru'
_chemical_formula_weight         802.81
_chemical_name_systematic
;

 ?

;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 118.417(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.1787(8)
_cell_length_b                   11.7916(5)
_cell_length_c                   19.3300(8)
_cell_measurement_reflns_used    9458
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      42.92
_cell_measurement_theta_min      2.41
_cell_volume                     3844.7(3)
_computing_cell_refinement       'Bruker SAINT-Plus v7.66A'
_computing_data_collection       'Bruker APEX2 v2009.7-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.66A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 23 settings'
_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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            274890
_diffrn_reflns_theta_full        43.69
_diffrn_reflns_theta_max         43.69
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  0.9223
_exptl_absorpt_correction_T_min  0.8670
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Deep purple'
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.427
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.059
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     479
_refine_ls_number_reflns         29175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.059
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0524
_reflns_number_gt                22486
_reflns_number_total             29175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4006966_si_002.cif
_cod_data_source_block           kje01
_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 2.4.2 from
2011-04-26.

'_refine_ls_weighting_scheme' value 'Sigma' changed to
'sigma' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4081414