Reactivity of an Unsaturated Iridium(III) Phosphoramidate Complex, [Cp*Ir{κ2-N,O}][BArF4]
Drover, Marcus W.; Johnson, Heather C.; Schafer, Laurel L.; Love, Jennifer A.; Weller, Andrew S.; Organometallics 34 (2015) 3849–; doi:10.1021/acs.organomet.5b00397

data_4087607
_publ_section_title
;
 Reactivity of an Unsaturated Iridium(III) Phosphoramidate Complex,
 [Cp*Ir{\k2-N,O}][BArF4]
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3849
_journal_paper_doi               10.1021/acs.organomet.5b00397
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety
'C32.04 H52.09 Ir N3 O3.02 P, C H2 Cl2, C32 H12 B F24'
_chemical_formula_sum            'C65.04 H66.09 B Cl2 F24 Ir N3 O3.02 P'
_chemical_formula_weight         1698.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.9224(10)
_cell_length_b                   24.6821(12)
_cell_length_c                   31.8660(16)
_cell_measurement_temperature    90
_cell_volume                     14096.3(13)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1366
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            112583
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.450
_diffrn_reflns_theta_min         1.543
_exptl_absorpt_coefficient_mu    2.103
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014) was used for absorption correction.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       plate
_exptl_crystal_F_000             6788
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.445
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         14475
_refine_ls_number_restraints     970
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0292P)^2^+59.7813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1113
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9282
_reflns_number_total             14475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00397_si_002.cif
_cod_data_source_block           3BARF
_cod_database_code               4087607
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F15-C65 = F16-C65 = F14-C65
 1.35 with sigma of 0.01
 O2-C13 \\sim O2A-C13A
 with sigma of 0.02
 O2-C13 \\sim O2A-C13A \\sim O2B-C13B
 with sigma of 0.02
 C14A-C13A \\sim C14-C13 \\sim C14B-C13B
 with sigma of 0.02
 C65A-C60 \\sim C65-C60 \\sim C64-C62
 with sigma of 0.02
 F14-F15 \\sim F15-F16 \\sim F16-F14
 with sigma of 0.01
 F14A-C65A \\sim F15A-C65A \\sim F16A-C65A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C14A) = Uanis(C14B) = Uanis(C14)
Uanis(C13) = Uanis(C13A) = Uanis(C13B)
Uanis(O2) = Uanis(O2A)
Uanis(C65) = Uanis(C65A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(O2)+Sof(C13)+Sof(H13A)+Sof(H13B)+Sof(C14)+Sof(H14D)+Sof(H14E)+
 Sof(H14F)]+1*[Sof(O2A)+Sof(C14A)+Sof(H14A)+Sof(H14B)+Sof(H14C)+Sof(C13A)+
 Sof(H13C)+Sof(H13D)]+1*[Sof(C13B)+Sof(H13E)+Sof(H13F)+Sof(C14B)+Sof(H14G)+
 Sof(H14H)+Sof(H14I)+Sof(O2B)]=1 with esd of 0.01
 Sof(O2)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14D)=Sof(H14E)=Sof(H14F)=
 FVAR(1)
 Sof(O2A)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C13A)=Sof(H13C)=
 Sof(H13D)=FVAR(2)
 Sof(C13B)=Sof(H13E)=Sof(H13F)=Sof(C14B)=Sof(H14G)=Sof(H14H)=Sof(H14I)=
 Sof(O2B)=FVAR(3)
 Sof(F16A)=Sof(F14A)=Sof(F15A)=Sof(C65A)=1-FVAR(4)
 Sof(C65)=Sof(F14)=Sof(F15)=Sof(F16)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C66(H66A,H66B), C13(H13A,H13B), C13A(H13C,H13D), C13B(H13E,H13F)
6.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C37(H37), C61(H61), C63(H63), C43(H43), C47(H47), C59(H59),
 C55(H55), C51(H51), C35(H35), C45(H45), C1AA(H1AA), C53(H53), C0AA(H0AA),
 C4(H4)
6.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C19(H19A,H19B,H19C), C029(H02A,H02B,H02C), C8(H8A,H8B,H8C), C7(H7A,H7B,
 H7C), C33(H33A,H33B,H33C), C22(H22A,H22B,H22C), C17(H17A,H17B,H17C), C10(H10A,
 H10B,H10C), C18(H18A,H18B,H18C), C23(H23A,H23B,H23C), C14A(H14A,H14B,H14C),
 C14(H14D,H14E,H14F), C14B(H14G,H14H,H14I)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'