A Tetracyclic Bis(imidazolindiylidene) Ligand and Its Diiridium and Dipalladium Complexes
Valdés, Hugo; Poyatos, Macarena; Peris, Eduardo; Organometallics 32 (2013) 6445–; doi:10.1021/om400779w

data_4081922
_publ_section_title
;
 A Tetracyclic Bis(imidazolindiylidene) Ligand and Its Diiridium and
 Dipalladium Complexes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6445
_journal_paper_doi               10.1021/om400779w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety
'2(C28 H42 Cl2 Ir2 N4), 2(C H Cl3), 0.5(C2 H4 Cl4)'
_chemical_formula_sum            'C59 H88 Cl12 Ir4 N8'
_chemical_formula_weight         2103.57
_chemical_name_systematic        str1516
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-07-29
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.9181(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1391(2)
_cell_length_b                   15.5045(3)
_cell_length_c                   31.8334(5)
_cell_measurement_reflns_used    18708
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      28.8300
_cell_measurement_theta_min      3.3770
_cell_volume                     7381.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.9190
_diffrn_measurement_details
;
  1 omega  -15.00   12.20   0.8000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  -99.0000  -90.0000 34

  2 omega  -55.00  -29.40   0.8000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  131.0000   99.0853 32

  3 omega  -16.00   26.40   0.8000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5252  -37.0000 -120.0000 53

  4 omega  -64.00   11.20   0.8000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5252  -77.0000    0.0000 94

  5 omega  -65.00  -33.00   0.8000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5252  -37.0000 -120.0000 40

  6 omega   71.00  101.40   0.8000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5252 -178.0000   90.0000 38

  7 omega    0.00   67.20   0.8000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5252 -121.0000  -73.2113 84

  8 omega   12.00   48.00   0.8000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5252  -77.0000   90.0000 45

  9 omega  -65.00  -23.40   0.8000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5252  -37.0000   30.0000 52

 10 omega  -22.00   98.00   0.8000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       14.5252   77.0000  -30.0000 150
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0393387000
_diffrn_orient_matrix_UB_12      0.0240830000
_diffrn_orient_matrix_UB_13      0.0012926000
_diffrn_orient_matrix_UB_21      0.0204485000
_diffrn_orient_matrix_UB_22      0.0373175000
_diffrn_orient_matrix_UB_23      -0.0070669000
_diffrn_orient_matrix_UB_31      -0.0169138000
_diffrn_orient_matrix_UB_32      -0.0109095000
_diffrn_orient_matrix_UB_33      -0.0213742000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            41054
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.196
_diffrn_reflns_theta_min         2.930
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.664
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_description       prism
_exptl_crystal_F_000             4040
_exptl_crystal_preparation
'Slow evaporation from a CHCl3/hexanes mixture'
_exptl_crystal_size_max          0.1678
_exptl_crystal_size_mid          0.1399
_exptl_crystal_size_min          0.0716
_refine_diff_density_max         9.652
_refine_diff_density_min         -1.589
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         9199
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+163.3679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1376
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7543
_reflns_number_total             9199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400779w_si_003.cif
_cod_data_source_block           str1516
_cod_database_code               4081922
_chemical_oxdiff_formula         'C28 H42 N4 Cl2 Ir2'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl7) \\sim Ueq, Uanis(Cl6) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Cl7(0.5) Cl6(0.5) C30(0.5) H30A(0.5) H30B(0.5)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C2(H2), C17(H17), C14(H14), C18(H18), C13(H13), C22(H22), C26(H26),
 C25(H25), C21(H21), C29(H29)
4.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C9(H9A,H9B), C8(H8A,H8B), C7(H7A,H7B), C28(H28A,H28B), C12(H12A,
 H12B), C27(H27A,H27B), C24(H24A,H24B), C23(H23A,H23B), C6(H6A,H6B), C15(H15A,
 H15B), C20(H20A,H20B), C16(H16A,H16B), C19(H19A,H19B), C10(H10A,H10B),
 C11(H11A,H11B), C30(H30A,H30B)
;
_shelx_hkl_checksum              83601
_shelx_res_checksum              56234
_shelxl_version_number           2013-4