Cationic Tris N-Heterocyclic Carbene Rhodium Carbonyl Complexes: Molecular Structures and Solution NMR Studies
Burling, Suzanne; Douglas, Susie; Mahon, Mary F.; Nama, Devendrababu; Pregosin, Paul S.; Whittlesey, Michael K.; Organometallics 25 (2006) 2642–; doi:10.1021/om060202p

data_4075316
_publ_section_title
;
 Cationic Tris N-Heterocyclic Carbene Rhodium Carbonyl Complexes:&#x00A0;
 Molecular Structures and Solution NMR Studies
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2642
_journal_paper_doi               10.1021/om060202p
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C34 H60 F6 N6 O P Rh'
_chemical_formula_weight         816.76
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           monoclinic
_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                80.367(1)
_cell_angle_beta                 76.200(1)
_cell_angle_gamma                80.032(1)
_cell_formula_units_Z            2
_cell_length_a                   9.9830(1)
_cell_length_b                   12.7140(1)
_cell_length_c                   16.4590(1)
_cell_measurement_reflns_used    60945
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.999
_cell_measurement_theta_min      1.018
_cell_volume                     1980.69(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'Denzo and Scalepack (otwinowski & Minor, 1997'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       KappaCCD
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40529
_diffrn_reflns_theta_full        30.91
_diffrn_reflns_theta_max         30.91
_diffrn_reflns_theta_min         3.56
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            Pale-yellow
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.0003(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         12310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+1.0142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                11164
_reflns_number_total             12310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060202psi20060324_021117.cif
_cod_data_source_block           c:\x-ray\helix\k05mkw6\maxus\k05mkw6
_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 2.4.1 from
2010-06-29.

'_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075316