Stable N-functionalised ‘pincer’ bis carbene ligands and their ruthenium complexes; synthesis and catalytic studies
Danopoulos, Andreas A.; Winston, Scott; Motherwell, William B.; Chemical Communications  (2002) 1376–; doi:10.1039/b202814j

data_7111216
_publ_section_title
;
 Stable N-functionalised &#x2018;pincer&#x2019; bis carbene ligands and
 their ruthenium complexes; synthesis and catalytic studies
;
_journal_issue                   13
_journal_name_full               'Chemical Communications'
_journal_page_first              1376
_journal_paper_doi               10.1039/b202814j
_journal_year                    2002
_chemical_formula_moiety         'C42.50 H53 N5 O'
_chemical_formula_sum            'C42.5 H53 N5 O'
_chemical_formula_weight         649.90
_chemical_name_common            02src088
_chemical_name_systematic
;
?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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            16
_cell_length_a                   29.947(2)
_cell_length_b                   48.760(4)
_cell_length_c                   10.9022(9)
_cell_measurement_reflns_used    7150
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      1.54
_cell_volume                     15920(2)
_computing_molecular_graphics    'Ortep 3 for windows (Farriga, 1997)'
_computing_publication_material  'Platon (Spek)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Smart CCD Area Detector'
_diffrn_measurement_method       'Phi and Omega scans to fill ewald sphere'
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       63
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17293
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.9997
_exptl_absorpt_correction_T_min  0.9993
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             5616
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.237
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   4(4)
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         7126
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_refine_ls_R_factor_gt           0.1115
_refine_ls_shift/su_max          1.098
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2992
_refine_ls_wR_factor_ref         0.3259
_reflns_number_gt                5712
_reflns_number_total             7126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202814jsup1.cif
_cod_data_source_block           compoundL1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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 
;
_cod_original_sg_symbol_H-M      Fdd2
_cod_original_formula_sum        'C42.50 H53 N5 O'
_cod_database_code               7111216