Oxidative Addition of the N‒H Bond of Ammonia to Iridium Bis(phosphane) Complexes: A Combined Experimental and Theoretical Study
Betoré, M. Pilar; Casado, Miguel A.; García-Orduña, Pilar; Lahoz, Fernando J.; Polo, Víctor; Oro, Luis A.; Organometallics 35 (2016) 720–; doi:10.1021/acs.organomet.5b01014

data_4086422
_publ_section_title
;
 Oxidative Addition of the N--H Bond of Ammonia to Iridium Bis(phosphane)
 Complexes: A Combined Experimental and Theoretical Study
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              720
_journal_paper_doi               10.1021/acs.organomet.5b01014
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety
'C77 H75 Ir2 N2 P6, 2(B F4), 2(C H2 Cl2), (C4 H10 O)'
_chemical_formula_sum            'C83 H89 B2 Cl4 F8 Ir2 N2 O P6'
_chemical_formula_weight         2016.20
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                88.7160(10)
_cell_angle_beta                 85.0540(10)
_cell_angle_gamma                68.5160(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8718(6)
_cell_length_b                   13.2090(6)
_cell_length_c                   25.6502(11)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.122
_cell_measurement_theta_min      2.235
_cell_volume                     4042.8(3)
_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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker APEX DUO CCD system'
_diffrn_measurement_method       'narrow \w frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            89019
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.599
_diffrn_reflns_theta_min         1.594
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.605
_exptl_absorpt_correction_T_max  0.6439
_exptl_absorpt_correction_T_min  0.4584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       plate
_exptl_crystal_F_000             2006
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.049
_platon_squeeze_details
;
The potential solvent accesible void volume (278.4 \A3) and the
electron count (73 e in the unit cell) may agree with the presence of two
ether molecules (C4 H10 O). 
;
_refine_diff_density_max         1.967
_refine_diff_density_min         -1.432
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         21211
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+4.3763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17867
_reflns_number_total             21211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b01014_si_001.cif
_cod_data_source_block           cmpnd_5
_cod_depositor_comments
'Adding full bibliography for 4086420--4086422.cif.'
_cod_database_code               4086422
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014-3
_shelx_res_checksum              14216
_shelx_hkl_checksum              69504