Cooperative Double Deprotonation of Bis(2-picolyl)amine Leading to Unexpected Bimetallic Mixed Valence (M-I, MI) Rhodium and Iridium Complexes
Cristina Tejel; M. Pilar del Río; Laura Asensio; Fieke J. van den Bruele; Miguel A. Ciriano; Nearchos Tsichlis i Spithas; Dennis G. H. Hetterscheid; Bas de Bruin; Inorganic Chemistry 50 (2011) 7524–7534; doi:10.1021/ic200395m

data_4325856
_publ_contact_author_address
;
 Dr. Cristina Tejel
 Departamento de Qu\'imica Inorg\'anica
 Instituto de Ciencia de Materiales de Arag\'on
 C.S.I.C.-Universidad de Zaragoza
 50009 Zaragoza, Spain
;
_publ_contact_author_email       ctejel@unizar.es
_publ_contact_author_fax         '+34 976 761187'
_publ_contact_author_name        'Dr. Cristina Tejel'
_publ_contact_author_phone       '+34 976 762285'
_publ_section_title
;
 Cooperative Double Deprotonation of Bis(2-picolyl)amine Leading to
 Unexpected Bimetallic Mixed Valence (M-I, MI) Rhodium and Iridium
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7524
_journal_page_last               7534
_journal_paper_doi               10.1021/ic200395m
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C28 H35 Ir2 N3, 0.5(C6 H14)'
_chemical_formula_sum            'C31 H42 Ir2 N3'
_chemical_formula_weight         841.08
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.8210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2335(8)
_cell_length_b                   12.1644(7)
_cell_length_c                   18.2294(10)
_cell_measurement_reflns_used    6140
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.07
_cell_measurement_theta_min      2.35
_cell_volume                     2742.9(3)
_computing_cell_refinement       'SAINT+ v. 7.56A (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 v. 4.0 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ v. 7.56A (Bruker AXS, 2008)'
_computing_molecular_graphics
;
ORTEP3 for Windows - L. J. Farrugia, 
J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_structure_refinement
;
SHELX97 - Programs for Crystal Structure Analysis (Release 97-2). 
G. M. Sheldrick, Institut fur Anorganische Chemie der Universitat, 
Tammanstrasse 4, D-3400 Gottingen, Germany, 1998.
;
_computing_structure_solution
;
SHELX97 - Programs for Crystal Structure Analysis (Release 97-2). 
G. M. Sheldrick, Institut fur Anorganische Chemie der Universitat, 
Tammanstrasse 4, D-3400 Gottingen, Germany, 1998.
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16938
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.06
_diffrn_source                   'normal-focus sealed tube'
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.718
_exptl_absorpt_correction_T_max  0.5502
_exptl_absorpt_correction_T_min  0.3583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
  SADABS-2008/1: Area-Detector Absorption Correction. Bruker-AXS 
;
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    2.037
_exptl_crystal_description       plate
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.760
_refine_diff_density_min         -1.634
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5947
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+4.8014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                4815
_reflns_number_total             5947
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200395m_si_002_2.cif
_cod_data_source_block           ctb113as
_cod_database_code               4325856