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_4082050
_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         '2(Cl), C30 H26 N4, 3(H2 O), 7(O)'
_chemical_formula_sum            'C30 H44 Cl2 N4 O10'
_chemical_formula_weight         691.59
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_symmetry_space_group_name_Hall  '-I 2yc'
_symmetry_space_group_name_H-M   'I 1 2/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 Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.1009(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6444(3)
_cell_length_b                   9.93793(18)
_cell_length_c                   21.1486(4)
_cell_measurement_reflns_used    7943
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      72.7360
_cell_measurement_theta_min      3.2670
_cell_volume                     3493.09(11)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9864
_diffrn_measurement_details
;
  1 omega  -78.00   25.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057   93.0000   89.0000 103

  2 omega  -94.00   -2.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -77.0000  -90.0000 92

  3 omega  -33.00    3.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000   30.0000  -90.0000 36

  4 omega  -23.00   12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000   30.0000   60.0000 35

  5 omega   55.00   84.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  -30.0000   30.0000 29

  6 omega   72.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   30.0000 -180.0000 106

  7 omega   38.00  103.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308 -111.0000   60.0000 65

  8 omega   30.00   87.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  -30.0000 -180.0000 57

  9 omega   32.00   84.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308 -111.0000 -120.0000 52

 10 omega   65.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  -94.0000  -90.0000 44

 11 omega   24.00  135.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  -77.0000   60.0000 111

 12 omega -116.00   -5.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -57.0000   90.0000 111

 13 omega -122.00   -2.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -77.0000    0.0000 120

 14 omega -153.00  -32.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000  -77.0000 -150.0000 121

 15 omega   70.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   30.0000  -30.0000 108

 16 omega   77.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   45.0000 -120.0000 101

 17 omega   75.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   61.0000   30.0000 103

 18 omega   27.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308 -111.0000 -180.0000 88

 19 omega   75.00  178.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   61.0000   90.0000 103

 20 omega -122.00   -2.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -77.0000 -120.0000 120

 21 omega   57.00   87.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       37.6057  178.0000    0.0000 30
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0138085000
_diffrn_orient_matrix_UB_12      0.0934196000
_diffrn_orient_matrix_UB_13      -0.0565175000
_diffrn_orient_matrix_UB_21      0.0333187000
_diffrn_orient_matrix_UB_22      -0.1195926000
_diffrn_orient_matrix_UB_23      -0.0368350000
_diffrn_orient_matrix_UB_31      -0.0853802000
_diffrn_orient_matrix_UB_32      -0.0315840000
_diffrn_orient_matrix_UB_33      -0.0277998000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16163
_diffrn_reflns_theta_full        72.65
_diffrn_reflns_theta_max         72.65
_diffrn_reflns_theta_min         4.19
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.169
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63627
_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     clear
_exptl_crystal_colour_modifier   whitish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0543
_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^)+(0.1339P)^2^+1.0872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.1868
_reflns_number_gt                2966
_reflns_number_total             3423
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400950d_si_002.cif
_cod_data_source_block           Compound_1
_cod_original_cell_volume        3493.10(11)
_cod_database_code               4082050
_chemical_oxdiff_formula         'C30 H26 N4 Cl2'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 O(H,H) groups
2. Others
 Fixed Sof: H23A(0.5) H23B(0.5)
3.a Free rotating group:
 O20(H20A,H20B), O23(H23A,H23B)
3.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C12(H12), C15(H15), C13(H13), C8(H8), C16(H16), C6(H6), C9(H9), C7(H7)
;