Synthesis and Properties of Compressed Dihydride Complexes of Iridium: Theoretical and Spectroscopic Investigations
Ricard Gelabert; Miquel Moreno; José M. Lluch; Agustí Lledós; Vincent Pons; Michael D. Heinekey; Journal of the American Chemical Society 126 (2004) 8813–8822; doi:10.1021/ja048775l

data_4112764
_publ_contact_author
;
Heinekey, Michael D.
Department of Chemistry, BOX 351700
University of Washington
Seattle, WA 98195
USA
;
_publ_contact_author_email       heinekey@chem.washington.edu
_publ_section_title
;
 Synthesis and Properties of Compressed Dihydride Complexes of Iridium:
 Theoretical and Spectroscopic Investigations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8813
_journal_page_last               8822
_journal_paper_doi               10.1021/ja048775l
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C15 H29 Cl Ir P2, C24 B F20'
_chemical_formula_sum            'C39 H29 B Cl F20 Ir P2'
_chemical_formula_weight         1178.02
_chemical_name_common            CpsIrdmpmCl
_chemical_name_systematic        '[Cp*Ir(dmpm)Cl][BArF4]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_method           SHELXL-97
_cell_angle_alpha                74.2690(18)
_cell_angle_beta                 80.1290(15)
_cell_angle_gamma                84.017(4)
_cell_formula_units_Z            2
_cell_length_a                   11.5620(4)
_cell_length_b                   12.2440(5)
_cell_length_c                   15.1400(8)
_cell_measurement_reflns_used    389
_cell_measurement_temperature    130(2)
_cell_volume                     2028.71(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.814
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_sigmaI/netI    0.1220
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11444
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    3.559
_exptl_absorpt_correction_T_max  0.509
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_description       prism
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.350
_refine_diff_density_min         -2.061
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         8265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                6201
_reflns_number_total             8265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048775lsi20040430_035439.cif
_cod_data_source_block           shelxl
_cod_database_code               4112764