Alcohol Amination with Aminoacidato Cp*Ir(III)-Complexes as Catalysts: Dissociation of the Chelating Ligand during Initiation
Wöckel, Simone; Plessow, Philipp; Schelwies, Mathias; Brinks, Marion K.; Rominger, Frank; Hofmann, Peter; Limbach, Michael; ACS Catalysis 4 (2014) 152–; doi:10.1021/cs4009418

data_4509840
_publ_section_title
;
 Alcohol Amination with Aminoacidato Cp*Ir(III)-Complexes as Catalysts:
 Dissociation of the Chelating Ligand during Initiation
;
_journal_issue                   1
_journal_name_full               'ACS Catalysis'
_journal_page_first              152
_journal_paper_doi               10.1021/cs4009418
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C10.5 H26 Cl2 Ir N3 O0.5'
_chemical_formula_weight         465.44
_chemical_name_common            '13 [Cp*Ir(NH3)3]Cl2 in manuscript'
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.1269(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.3281(6)
_cell_length_b                   13.3359(7)
_cell_length_c                   24.1586(14)
_cell_measurement_reflns_used    6069
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.65
_cell_measurement_theta_min      2.50
_cell_volume                     3318.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20464
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.735
_diffrn_reflns_theta_min         1.977
_exptl_absorpt_coefficient_mu    8.357
_exptl_absorpt_correction_T_max  0.5492
_exptl_absorpt_correction_T_min  0.4420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen, Germany.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.225
_refine_diff_density_min         -1.503
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6723
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+38.1431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5673
_reflns_number_total             6723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs4009418_si_002.cif
_cod_data_source_block           siw13
_cod_original_formula_sum        'C10.50 H26 Cl2 Ir N3 O0.50'
_cod_database_code               4509840
_shelx_estimated_absorpt_t_min   0.460
_shelx_estimated_absorpt_t_max   0.489
_shelxl_version_number           2013-3
_shelx_res_checksum              45918
_shelx_hkl_checksum              65369