Rhodium Complexes of a Chelating Ligand with Imidazol-2-ylidene and Pyridin-2-ylidene Donors: The Effect of C-Metalation of Nicotinamide Groups on Uptake of Hydride Ion
Alex McSkimming; Graham E. Ball; Mohan M. Bhadbhade; Stephen B. Colbran; Inorganic Chemistry 51 (2012) 2191–2203; doi:10.1021/ic202164v

data_4328327
_publ_section_title
;
 Rhodium Complexes of a Chelating Ligand with Imidazol-2-ylidene and
 Pyridin-2-ylidene Donors: The Effect of C-Metalation of Nicotinamide
 Groups on Uptake of Hydride Ion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2191
_journal_page_last               2203
_journal_paper_doi               10.1021/ic202164v
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C56 H53 I2 N4 O3 Rh, C2 H3 N'
_chemical_formula_sum            'C58 H56 I2 N5 O3 Rh'
_chemical_formula_weight         1227.79
_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                102.685(5)
_cell_angle_beta                 96.435(5)
_cell_angle_gamma                110.518(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5255(11)
_cell_length_b                   13.6554(16)
_cell_length_c                   19.825(3)
_cell_measurement_reflns_used    2470
_cell_measurement_temperature    184(2)
_cell_measurement_theta_max      21.740
_cell_measurement_theta_min      2.389
_cell_volume                     2547.2(6)
_computing_cell_refinement       '<i>APEX2 </i>(Bruker, 2007)'
_computing_data_collection       '<i>APEX2 </i>(Bruker, 2007)'
_computing_data_reduction        '<i>APEX2 </i>(Bruker, 2007)'
_computing_molecular_graphics    '<i>SHELXTL-Plus</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL-97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      184(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.1112
_diffrn_reflns_av_sigmaI/netI    0.1640
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28342
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    1.598
_exptl_absorpt_correction_T_max  0.9521
_exptl_absorpt_correction_T_min  0.7944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         8960
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1565
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0423P)^2^+1.6002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                4263
_reflns_number_total             8960
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202164v_si_007.cif
_cod_data_source_block           inp1bar
_cod_original_cell_volume        2547.2(5)
_cod_database_code               4328327