Coordination Singularities of a Bis(p-xylyl)bis(benzimidazolylidene) Ligand and the Bis-iridium and -rhodium-Related Complexes
Ruiz-Botella, Sheila; Guisado-Barrios, Gregorio; Mata, José A.; Peris, Eduardo; Organometallics 32 (2013) 6613–; doi:10.1021/om400950d

data_4082051
_publ_section_title
;
 Coordination Singularities of a Bis(p-xylyl)bis(benzimidazolylidene)
 Ligand and the Bis-iridium and -rhodium-Related Complexes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6613
_journal_paper_doi               10.1021/om400950d
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C50 H54 Cl4 Ir2 N4, C H2 Cl2, C H4 O, O'
_chemical_formula_sum            'C52 H60 Cl6 Ir2 N4 O'
_chemical_formula_weight         1354.14
_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             2013-10-08
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.9727(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.3681(4)
_cell_length_b                   14.0701(3)
_cell_length_c                   18.2729(4)
_cell_measurement_reflns_used    24876
_cell_measurement_temperature    200.05(10)
_cell_measurement_theta_max      28.7460
_cell_measurement_theta_min      3.2020
_cell_volume                     5493.0(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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      200.05(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.9019
_diffrn_measurement_details
;
  1 omega -100.00  -60.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  178.0000    0.0000 40

  2 omega  -81.00  -54.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -37.0000 -180.0000 27

  3 omega   -8.00   19.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253   57.0000   30.0000 27

  4 omega   43.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  178.0000  150.0000 45

  5 omega   -5.00   46.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  -77.0000    0.0000 51

  6 omega   52.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191   37.0000  -90.0000 32

  7 omega  -62.00  -36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  -77.0000    0.0000 26

  8 omega   70.00  102.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191    0.0000  -30.0000 32

  9 omega  -77.00   11.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191    0.0000  -30.0000 88

 10 omega  -64.00   19.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  -37.0000 -150.0000 83
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0280573000
_diffrn_orient_matrix_UB_12      0.0232111000
_diffrn_orient_matrix_UB_13      -0.0100076000
_diffrn_orient_matrix_UB_21      0.0017437000
_diffrn_orient_matrix_UB_22      -0.0290501000
_diffrn_orient_matrix_UB_23      -0.0316044000
_diffrn_orient_matrix_UB_31      -0.0176892000
_diffrn_orient_matrix_UB_32      0.0339730000
_diffrn_orient_matrix_UB_33      -0.0202372000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61595
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.81
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70584
_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
;
;
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.765
_refine_diff_density_min         -2.480
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         12437
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0684P)^2^+32.5766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1412
_reflns_number_gt                10466
_reflns_number_total             12437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400950d_si_002.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        5492.97(19)
_cod_database_code               4082051
_chemical_oxdiff_formula         'C50 H54 N4 Cl4 Ir2'
_reflns_odcompleteness_completeness 99.80
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C9(H9A,H9B), C39(H39A,H39B), C32(H32A,H32B), C65(H65A,H65B)
3.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C15(H15), C13(H13), C23(H23), C14(H14), C27(H27), C31(H31),
 C28(H28), C21(H21), C38(H38), C24(H24), C30(H30), C34(H34), C35(H35), C12(H12),
  C37(H37)
3.c Tetrahedral OH refined with riding coordinates:
 O1(H1)
3.d Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C43(H43A,H43B,H43C), C41(H41A,H41B,H41C), C45(H45A,H45B,
 H45C), C57(H57A,H57B,H57C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C51(H51A,
 H51B,H51C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C2(H2A,H2B,H2C)
;