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_4082052
_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         'C46 H48 Cl2 N4 Rh2, C4 H10 O'
_chemical_formula_sum            'C50 H58 Cl2 N4 O Rh2'
_chemical_formula_weight         1007.72
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-18
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2013.07.16 svn.r0, GUI svn.r4533)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.9457(3)
_cell_length_b                   19.1797(4)
_cell_length_c                   23.0383(5)
_cell_measurement_reflns_used    8414
_cell_measurement_temperature    200.1(3)
_cell_measurement_theta_max      60.9670
_cell_measurement_theta_min      3.6250
_cell_volume                     9255.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      200.1(3)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.9861
_diffrn_measured_fraction_theta_max 0.9699
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0064528000
_diffrn_orient_matrix_UB_12      -0.0081364000
_diffrn_orient_matrix_UB_13      0.0662852000
_diffrn_orient_matrix_UB_21      -0.0235931000
_diffrn_orient_matrix_UB_22      0.0754149000
_diffrn_orient_matrix_UB_23      0.0083329000
_diffrn_orient_matrix_UB_31      -0.0693311000
_diffrn_orient_matrix_UB_32      -0.0264429000
_diffrn_orient_matrix_UB_33      0.0033757000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18009
_diffrn_reflns_theta_full        61.03
_diffrn_reflns_theta_max         61.03
_diffrn_reflns_theta_min         3.67
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.141
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.241
_refine_diff_density_min         -1.496
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         6913
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1175P)^2^+32.7438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2151
_reflns_number_gt                5926
_reflns_number_total             6913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400950d_si_002.cif
_cod_data_source_block           compound_3
_cod_database_code               4082052
_chemical_oxdiff_formula         'C46 H48 Cl2 N4 Rh2'
_chemical_oxdiff_usercomment     SR230
_reflns_odcompleteness_completeness 98.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_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
2. Restrained distances
 C58-C59
 1.4 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C40(H40), C43(H43), C47(H47), C52(H52), C44(H44), C39(H39), C48(H48), C51(H51)
3.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C42(H42A,H42B), C31(H31A,H31B), C23(H23A,H23B), C38(H38A,
 H38B), C53(H53A,H53B), C50(H50A,H50B), C46(H46A,H46B), C49(H49A,H49B),
 C54(H54A,H54B), C45(H45A,H45B), C41(H41A,H41B), C56(H56A,H56B), C58(H58A,H58B)
3.c Me refined with riding coordinates:
 C59(H59A,H59B,H59C)
3.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C26(H26), C13(H13), C28(H28), C27(H27), C36(H36),
 C25(H25), C33(H33), C35(H35), C34(H34), C20(H20), C22(H22), C21(H21), C19(H19),
  C12(H12)
3.e Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C)
;