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_4331051
_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         'Ir C20 H29 N O3 P F6'
_chemical_formula_sum            'C20 H29 F6 Ir N O3 P'
_chemical_formula_weight         668.64
_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                 98.978(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   7.9352(15)
_cell_length_b                   18.617(4)
_cell_length_c                   16.983(3)
_cell_measurement_reflns_used    14476
_cell_measurement_temperature    223
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      3.04
_cell_volume                     2478.2(8)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalClear
_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      223
_diffrn_detector_area_resol_mean 6.849
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  SCX-MINI
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20099
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.532
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1304.00
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.610
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4676
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0238P)^2^+2.7848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0791
_reflns_number_gt                3717
_reflns_number_total             4821
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic301601c_si_002_6.cif
_cod_data_source_block           4
_cod_original_formula_sum        'Ir C20 H29 N O3 P F6'
_cod_database_code               4331051