Dehydrogenation of Cyclic Amines by a Coordinatively Unsaturated Cp*Ir(III) Phosphoramidate Complex
Drover, Marcus W.; Schafer, Laurel L.; Love, Jennifer; Dalton Trans.  (2017) –; doi:10.1039/C7DT01499F

data_7043189
_publ_section_title
;
 Dehydrogenation of Cyclic Amines by a Coordinatively Unsaturated
 Cp*Ir(III) Phosphoramidate Complex
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01499F
_journal_year                    2017
_chemical_formula_moiety         'C15 H26 Cl2 Ir N'
_chemical_formula_sum            'C15 H26 Cl2 Ir N'
_chemical_formula_weight         483.47
_chemical_name_systematic        '[Cp*Ir(NH(CH2)3CH2CH2)(Cl)2]'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-05
_audit_creation_method
;
Olex2 1.2
(compiled Jan 19 2015 12:28:14 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-03-09 deposited with the CCDC.
2017-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.981(3)
_cell_length_b                   13.452(3)
_cell_length_c                   9.6850(13)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      22.724
_cell_measurement_theta_min      5.551
_cell_volume                     1691.2(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8634
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.156
_diffrn_reflns_theta_min         2.591
_exptl_absorpt_coefficient_mu    8.199
_exptl_absorpt_correction_T_max  0.4781
_exptl_absorpt_correction_T_min  0.2743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1049 before and 0.0571 after correction.
The Ratio of minimum to maximum transmission is 0.5737.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.864
_refine_diff_density_min         -2.120
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0196P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1915
_reflns_number_total             2353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01499f2.cif
_cod_data_source_block           noncentro
_cod_original_cell_volume        1691.2(5)
_cod_database_code               7043189
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H4A(0.5) H4C(0.5) H4B(0.5)
3.a Ternary CH refined with riding coordinates:
 N1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7B,H7A), C8(H8A,H8B), C9(H9A,H9B)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4C,H4B), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              58374
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'