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_4082053
_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         'C32 H25 Cl N4 O3 Rh2, C H2 Cl2'
_chemical_formula_sum            'C33 H27 Cl3 N4 O3 Rh2'
_chemical_formula_weight         839.76
_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             2013-09-23
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                87.0246(14)
_cell_angle_beta                 89.5385(16)
_cell_angle_gamma                61.383(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3896(2)
_cell_length_b                   9.56605(18)
_cell_length_c                   19.5108(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1536.05(6)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.894
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29137
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         3.12
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.378
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             836
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0206P)^2^+3.4037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                5712
_reflns_number_total             6758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400950d_si_002.cif
_cod_data_source_block           compound_5
_cod_original_cell_volume        1536.05(5)
_cod_database_code               4082053
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C43(H43A,H43B), C42(H42A,H42B), C35(H35A,H35B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C12(H12), C20(H20), C38(H38), C24(H24), C37(H37), C41(H41),
 C15(H15), C30(H30), C31(H31), C40(H40), C14(H14), C13(H13), C23(H23), C33(H33),
  C32(H32)
;