Di-Mesoionic Carbene-Bridged Complexes of Rh2, Ir2, and RhIr: A Stepwise Metalation Strategy for the Synthesis of di-MIC-Bridged Mixed-Metal Systems
Zamora, Matthew T.; Ferguson, Michael J.; Cowie, Martin; Organometallics 31 (2012) 5384–; doi:10.1021/om300423z

data_4078786
_publ_section_title
;
 Di-Mesoionic Carbene-Bridged Complexes of Rh2, Ir2, and RhIr: A Stepwise
 Metalation Strategy for the Synthesis of di-MIC-Bridged Mixed-Metal
 Systems
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              5384
_journal_paper_doi               10.1021/om300423z
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C52 H68 I2 N6 Rh2, 0.75(C2 H3 N)'
_chemical_formula_sum            'C53.5 H70.25 I2 N6.75 Rh2'
_chemical_formula_weight         1267.53
_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                69.8435(9)
_cell_angle_beta                 85.4295(11)
_cell_angle_gamma                89.9816(12)
_cell_formula_units_Z            2
_cell_length_a                   11.0441(2)
_cell_length_b                   15.0942(3)
_cell_length_c                   17.8573(4)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.54
_cell_measurement_theta_min      3.12
_cell_volume                     2784.47(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18784
_diffrn_reflns_theta_full        67.80
_diffrn_reflns_theta_max         69.58
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    13.792
_exptl_absorpt_correction_T_max  0.4496
_exptl_absorpt_correction_T_min  0.1730
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1269
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.482
_refine_diff_density_min         -2.338
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9835
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0704
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+22.8160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1732
_reflns_number_gt                8450
_reflns_number_total             9835
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300423z_si_003.cif
_cod_data_source_block           7
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_formula_sum        'C53.50 H70.25 I2 N6.75 Rh2'
_cod_database_code               4078786