Conformations of N-Heterocyclic Carbene Ligands in Ruthenium Complexes Relevant to Olefin Metathesis
Ian C. Stewart; Diego Benitez; Daniel J. O'Leary; Ekaterina Tkatchouk; Michael W. Day; William A. Goddard; Robert H. Grubbs; Journal of the American Chemical Society 131 (2009) 1931–1938; doi:10.1021/ja8078913

data_4103884
_publ_section_title
;
 Conformations of N-Heterocyclic Carbene Ligands in Ruthenium Complexes
 Relevant to Olefin Metathesis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1931
_journal_page_last               1938
_journal_paper_doi               10.1021/ja8078913
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C26 H26 Cl2 N2 Ru, C H2 Cl2'
_chemical_formula_sum            'C27 H28 Cl4 N2 Ru'
_chemical_formula_weight         623.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.1288(9)
_cell_length_b                   15.8049(8)
_cell_length_c                   19.8610(12)
_cell_measurement_reflns_used    9305
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      41.18
_cell_measurement_theta_min      2.58
_cell_volume                     5376.7(5)
_computing_cell_refinement       'Bruker SAINT-Plus v7.34A'
_computing_data_collection       'Bruker APEX2 v2.1-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.34A'
_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 0.993
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            195437
_diffrn_reflns_theta_full        36.74
_diffrn_reflns_theta_max         42.01
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_T_max  0.8645
_exptl_absorpt_correction_T_min  0.7403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'Pale green'
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.773
_refine_diff_density_min         -2.082
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.35(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.288
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     684
_refine_ls_number_reflns         33122
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      2.317
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.003
_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          0.0956
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                19451
_reflns_number_total             33122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8078913_si_003.cif
_cod_data_source_block           ics04_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'Sigma' changed to 'sigma'
according to the built-in table from CIF Core 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 

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_Hall     P2c-2ac
_cod_database_code               4103884