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_4078904
_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         'C15 H19 I2 Ir N5, I, C2 H3 N'
_chemical_formula_sum            'C17 H22 I3 Ir N6'
_chemical_formula_weight         883.31
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2011-12-18
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                107.112(4)
_cell_angle_beta                 94.167(4)
_cell_angle_gamma                112.461(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1810(6)
_cell_length_b                   11.0855(5)
_cell_length_c                   12.6852(7)
_cell_measurement_reflns_used    8572
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      29.3618
_cell_measurement_theta_min      2.7197
_cell_volume                     1236.42(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_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      220.00(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details
;
  1 omega  -21.00   22.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.2867  -80.0000  164.0000 43

  2 omega  -63.00   18.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9899  -37.0000  -90.0000 81

  3 omega  -19.00   54.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9899  -99.0000 -180.0000 73

  4 omega  -45.00  -17.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9899  -80.0000 -107.0000 28

  5 omega  -18.00   77.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9899   57.0000   60.0000 95

  6 omega  -90.00   22.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.2867  -77.0000 -150.0000 112

  7 omega  -46.00   24.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.2867   80.0000  107.0000 70

  8 omega -100.00  -55.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.2867  178.0000 -180.0000 45

  9 omega  -87.00   15.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.2867  -37.0000   30.0000 102

 10 omega  -14.00   88.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9899   37.0000    0.0000 102

 11 omega  -20.00   21.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9899  -99.0000  -30.0000 41

 12 omega   34.00  100.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       11.9899 -178.0000  120.0000 66
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0509194000
_diffrn_orient_matrix_UB_12      0.0077085000
_diffrn_orient_matrix_UB_13      -0.0356182000
_diffrn_orient_matrix_UB_21      -0.0426239000
_diffrn_orient_matrix_UB_22      -0.0694484000
_diffrn_orient_matrix_UB_23      -0.0368712000
_diffrn_orient_matrix_UB_31      -0.0391753000
_diffrn_orient_matrix_UB_32      0.0240331000
_diffrn_orient_matrix_UB_33      -0.0308538000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27397
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.43
_diffrn_reflns_theta_min         2.73
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    9.158
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.766
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         6297
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0515P)^2^+5.5796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                4264
_reflns_number_total             6297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3005096_si_005.cif
_cod_data_source_block           str1276
_cod_original_cell_volume        1236.42(11)
_cod_database_code               4078904
_chemical_oxdiff_formula         'C17 H23 N6 I4 Ir'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32