Rhodium and Iridium Complexes with ChelatingC‒C′-Imidazolylidene‒Pyridylidene Ligands: Systematic Approach to Normal, Abnormal, and Remote Coordination Modes
Segarra, Candela; Mas-Marzá, Elena; Mata, José A.; Peris, Eduardo; Organometallics 31 (2012) 5169–; doi:10.1021/om3005096

data_4078903
_publ_section_title
;
 Rhodium and Iridium Complexes with
 ChelatingC--C&#x2032;-Imidazolylidene--Pyridylidene Ligands: Systematic
 Approach to Normal, Abnormal, and Remote Coordination Modes
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              5169
_journal_paper_doi               10.1021/om3005096
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C14 H17 I2 N5 Rh, I'
_chemical_formula_sum            'C14 H17 I3 N5 Rh'
_chemical_formula_weight         738.94
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-04
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.612(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3673(4)
_cell_length_b                   24.5851(7)
_cell_length_c                   7.6286(3)
_cell_measurement_reflns_used    9020
_cell_measurement_temperature    199.95(10)
_cell_measurement_theta_max      29.3592
_cell_measurement_theta_min      2.7110
_cell_volume                     2095.47(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      199.95(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_details
;
  1 omega  -86.00  -60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.3597  178.0000    0.0000 26

  2 omega  -19.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.3597  -99.0000 -180.0000 48

  3 omega  -12.00   58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0628  -19.0000   90.0000 70

  4 omega   -6.00   36.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0628   38.0000   30.0000 42

  5 omega  -58.00  -25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0628  -19.0000   90.0000 33

  6 omega  -18.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0628   57.0000  120.0000 104

  7 omega  -67.00  -15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0628  -77.0000   30.0000 52

  8 omega   35.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0628  178.0000   30.0000 67
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0092965000
_diffrn_orient_matrix_UB_12      0.0266892000
_diffrn_orient_matrix_UB_13      0.0352382000
_diffrn_orient_matrix_UB_21      -0.0540802000
_diffrn_orient_matrix_UB_22      0.0086211000
_diffrn_orient_matrix_UB_23      -0.0547341000
_diffrn_orient_matrix_UB_31      -0.0318597000
_diffrn_orient_matrix_UB_32      -0.0068339000
_diffrn_orient_matrix_UB_33      0.0686112000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            24019
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.42
_diffrn_reflns_theta_min         2.84
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    5.240
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.466
_refine_diff_density_min         -2.300
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         5217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0387P)^2^+13.9582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                4031
_reflns_number_total             5217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3005096_si_004.cif
_cod_data_source_block           str1300
_cod_original_cell_volume        2095.48(12)
_cod_database_code               4078903
_chemical_oxdiff_formula         'C14 H14 N5 I3 Rh'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32