Reactivity of Parent Amido Complexes of Iridium with Olefins: C-NH2 Bond Formation versus C-H Activation
Casado, Miguel Ángel; Mena, Inmaculada; García-Orduña, Pilar; Polo, Victor; Lahoz, Fernando J.; Oro, Luis A.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01924F

data_7043859
_publ_section_title
;
 Reactivity of Parent Amido Complexes of Iridium with Olefins: C-NH2 Bond
 Formation versus C-H Activation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01924F
_journal_year                    2017
_chemical_formula_moiety         'C105 H94 F8 IR2 N2 P6, 5(C7 H8)'
_chemical_formula_sum            'C140 H134 F8 Ir2 N2 P6'
_chemical_formula_weight         2566.70
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-03-15 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   44.924(2)
_cell_length_b                   47.578(2)
_cell_length_c                   21.0515(11)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.744
_cell_measurement_theta_min      2.302
_cell_volume                     44995(4)
_computing_cell_refinement
'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction
'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX CCD system'
_diffrn_measurement_method       'narrow \w frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       63
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            129633
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         28.783
_diffrn_reflns_theta_min         1.712
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.518
_exptl_absorpt_correction_T_max  0.7768
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       prism
_exptl_crystal_F_000             20864
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.118
_platon_squeeze_details
;

SQUEEZE program has been used to calculated and correct for
density identified in the solvent accessible areas. 
The total potential solvent void (4890 A^3 /unit cell) and
the electron count (1936 e) agree with the presence of
two additional toluene molecules in the asymetric unit.

;
_refine_diff_density_max         1.394
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Flack x determined using 8996 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1136
_refine_ls_number_reflns         26983
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+85.4360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.891
_reflns_number_gt                22357
_reflns_number_total             26983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01924f2.cif
_cod_data_source_block           cmpnd_4
_cod_original_cell_volume        44996(4)
_cod_database_code               7043859
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014-3
_shelx_res_checksum              84398
_shelx_fab_checksum              95538