Activation of ethylene and ammonia at iridium: C‒H versus N‒H oxidative addition
Salomon, Marcel Ahijado; Jungton, Ann-Katrin; Braun, Thomas; Dalton Transactions  (2009) 7669–7677; doi:10.1039/b906189d

data_7002254
_publ_section_title
;
 Activation of ethylene and ammonia at iridium: C--H versus N--H
 oxidative addition
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              7669
_journal_page_last               7677
_journal_paper_doi               10.1039/b906189d
_journal_year                    2009
_chemical_formula_moiety         'C29 H50 F4 Ir N O4 P2'
_chemical_formula_sum            'C29 H50 F4 Ir N O4 P2'
_chemical_formula_weight         806.84
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7834(16)
_cell_length_b                   14.3514(16)
_cell_length_c                   21.382(3)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     3309.0(8)
_computing_cell_refinement       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_collection       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_reduction        'IPDS2.87 (Stoe & Cie, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Stoe IPDS diffractometer'
_diffrn_measurement_method       '\f-rotation,\f-incr.=1.2\%,180 exposures'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32822
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.187
_exptl_absorpt_correction_T_max  0.7305
_exptl_absorpt_correction_T_min  0.4331
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The program XSHAPE1.02 (Stoe, 1997) was used for crystal optimisation
before the numerical absorption correction basing on a Gaussian algorithsm
and implemented in XRED1.08 (Stoe, 1997) was applied.
In XSHAPE 150 strong reflections with 4 symmetry equivalents in each case
were used for that optimisation. XSHAPE bases on the program HABITUS
(Herrendorf, W. (1993). PhD thesis. Universit\"at Karlsruhe, Germany).
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(3)
_refine_ls_extinction_coef       0.00013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0098P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0272
_refine_ls_wR_factor_ref         0.0276
_reflns_number_gt                5505
_reflns_number_total             6150
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b906189d.txt
_cod_data_source_block           akju6_complex4
_cod_original_cell_volume        3309.0(7)
_cod_database_code               7002254