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_4063879
_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
'C60 H57 N2 O3 Os P4 Rh, 2(C F3 O3 S), 2(C H2 Cl2)'
_chemical_formula_sum            'C64 H61 Cl4 F6 N2 O9 Os P4 Rh S2'
_chemical_formula_weight         1739.06
_chemical_name_systematic
; 
 ? 
;
_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                87.0519(11)
_cell_angle_beta                 71.6752(10)
_cell_angle_gamma                79.8666(10)
_cell_formula_units_Z            2
_cell_length_a                   13.6192(10)
_cell_length_b                   13.9648(10)
_cell_length_c                   20.2106(14)
_cell_measurement_reflns_used    6432
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.23
_cell_volume                     3592.0(4)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27157
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.362
_exptl_absorpt_correction_T_max  0.6368
_exptl_absorpt_correction_T_min  0.3674
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as solvent
dichloromethane chlorine or carbon atoms were unsuccessful.  The data were
corrected for disordered electron density through use of the SQUEEZE
procedure (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46,
194-201) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46,
C34.  PLATON - a multipurpose crystallographic tool.  Utrecht University,
Utrecht, The Netherlands).  A total solvent-accessible void volume of
661.5 cubic Angstroms with a total electron count of 102 was found in the
unit cell, consistent with four molecules of solvent dichloromethane in
the cell, or two molecules of dichloromethane per formula unit of the
complex dication.
;
_refine_diff_density_max         1.228
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         14577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.9563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                12962
_reflns_number_total             14577
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om1010066_si_003.cif
_cod_data_source_block           19b
_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_database_code               4063879