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_7002256
_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         'C20 H32 F4 Ir N2 O4 P, 0.5(C6 H6)'
_chemical_formula_sum            'C23 H35 F4 Ir N2 O4 P'
_chemical_formula_weight         702.70
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.780(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7892(4)
_cell_length_b                   10.4836(2)
_cell_length_c                   17.1372(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     2625.89(13)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Stoe IPDS-2t diffractometer'
_diffrn_measurement_method       '\w-rotation,\w-incr.=1\%,360 exposures'
_diffrn_radiation_collimation    '0.5 mm diameter monocapillary'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'long fine focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0952
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47604
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.205
_exptl_absorpt_correction_T_max  0.3235
_exptl_absorpt_correction_T_min  0.2559
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The crystal faces were indexed by microscope on the diffractometer. After
that a numerical absorption correction basing on a Gaussian algorithsm
was applied, which is implemented in the X-RED program (Stoe, 2002).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.545
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.00202(9)
_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   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6817
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0415
_reflns_number_gt                5946
_reflns_number_total             6817
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b906189d.txt
_cod_data_source_block           akju13_complex6
_cod_original_cell_volume        2625.89(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7002256