Influences of N-Heterocyclic Carbene and PMe3Ligands on the Tautomerism between Methylene/Hydride and Bridging Methyl Complexes of Rh/Os and Unusual Examples of Ligand Deprotonation by the NHC Group
Wells, Kyle D.; McDonald, Robert; Ferguson, Michael J.; Cowie, Martin; Organometallics 30 (2011) 2654–; doi:10.1021/om1010066

data_4063878
_publ_section_title
;
 Influences of N-Heterocyclic Carbene and PMe3Ligands on the Tautomerism
 between Methylene/Hydride and Bridging Methyl Complexes of Rh/Os and
 Unusual Examples of Ligand Deprotonation by the NHC Group
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2654
_journal_paper_doi               10.1021/om1010066
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety
'C56 H53 O3 Os P5 Rh, C F3 O3 S, 1.25(C H2 Cl2)'
_chemical_formula_sum            'C58.25 H55.5 Cl2.5 F3 O6 Os P5 Rh S'
_chemical_formula_weight         1477.17
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.1200(18)
_cell_angle_beta                 106.6178(18)
_cell_angle_gamma                108.1151(17)
_cell_formula_units_Z            2
_cell_length_a                   12.7428(17)
_cell_length_b                   15.891(2)
_cell_length_c                   17.468(2)
_cell_measurement_reflns_used    6208
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.484
_cell_measurement_theta_min      2.420
_cell_volume                     3205.3(7)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14437
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    2.553
_exptl_absorpt_correction_T_max  0.8028
_exptl_absorpt_correction_T_min  0.3559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, v 1.05'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
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_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.551
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         14437
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0986P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1490
_reflns_number_gt                11542
_reflns_number_total             14437
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om1010066_si_003.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        3205.2(7)
_cod_database_code               4063878