Symmetrical Hydrogen Bonds in Iridium(III) Alkoxides with Relevance to Outer Sphere Hydrogen Transfer
Nathan D. Schley; Stéphanie Halbert; Christophe Raynaud; Odile Eisenstein; Robert H. Crabtree; Inorganic Chemistry 51 (2012) 12313–12323; doi:10.1021/ic301601c

data_4331053
_publ_contact_author_address
;    Department of Chemistry
     Yale University
     225 Prospect St
     PO Box 208107
     New Haven, CT 06520-8107
     USA
;
_publ_contact_author_email       robert.crabtree@yale.edu
_publ_contact_author_fax         '+203 432 6144'
_publ_contact_author_name        'Dr. Robert H Crabtree'
_publ_contact_author_phone       '+203 432 3925'
_publ_section_title
;
 Symmetrical Hydrogen Bonds in Iridium(III) Alkoxides with Relevance to
 Outer Sphere Hydrogen Transfer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12313
_journal_page_last               12323
_journal_paper_doi               10.1021/ic301601c
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'Ir2 C50 H68 N2 O2 P2 F12'
_chemical_formula_sum            'C50 H68 F12 Ir2 N2 O2 P2'
_chemical_formula_weight         1403.47
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 110.182(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   18.5780(3)
_cell_length_b                   13.3039(2)
_cell_length_c                   22.7037(16)
_cell_measurement_reflns_used    42000
_cell_measurement_temperature    93
_cell_measurement_theta_max      65.17
_cell_measurement_theta_min      2.54
_cell_volume                     5266.9(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 11.111
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  Saturn994
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60177
_diffrn_reflns_theta_full        65.08
_diffrn_reflns_theta_max         65.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.721
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       prism
_exptl_crystal_F_000             2760.00
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.950
_refine_diff_density_min         -1.720
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     717
_refine_ls_number_reflns         8823
_refine_ls_number_restraints     259
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0543P)^2^+37.0008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1320
_reflns_number_gt                7444
_reflns_number_total             9211
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic301601c_si_002_8.cif
_cod_data_source_block           6
_cod_original_formula_sum        'Ir2 C50 H68 N2 O2 P2 F12'
_cod_database_code               4331053