Iridium(III) Hydrido N-Heterocyclic Carbene-Phosphine Complexes as Catalysts in Magnetization Transfer Reactions
Marianna Fekete; Oliver Bayfield; Simon B. Duckett; Sam Hart; Ryan E. Mewis; Natalie Pridmore; Peter J. Rayner; Adrian Whitwood; Inorganic Chemistry 52 (2013) 13453–13461; doi:10.1021/ic401783c

data_4336814
_publ_contact_author_name
;
;
_publ_section_title
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 Iridium(III) Hydrido N-Heterocyclic Carbene-Phosphine Complexes as
 Catalysts in Magnetization Transfer Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13453
_journal_page_last               13461
_journal_paper_doi               10.1021/ic401783c
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'B F4, C46 H49 Ir N4 P, C6 H6'
_chemical_formula_sum            'C52 H55 B F4 Ir N4 P'
_chemical_formula_weight         1045.98
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-02-01
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.8105(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.48681(16)
_cell_length_b                   16.4667(3)
_cell_length_c                   15.8574(3)
_cell_measurement_reflns_used    12279
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      32.1005
_cell_measurement_theta_min      2.8087
_cell_volume                     2371.33(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
Palatinus, L. & Chapuis, G. (2007).
SUPERFLIP - a computer program for the solution of crystal structures
 by charge flipping in arbitrary dimensions.
J. Appl. Cryst. 40, 786-790.
;
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9956
_diffrn_measured_fraction_theta_max 0.9848
_diffrn_measurement_details
;
  1 omega   -2.00   24.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1672   19.0000   60.0000 26

  2 omega  -46.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172    0.0000 -150.0000 129

  3 omega   48.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172  178.0000 -120.0000 50

  4 omega  -94.00  -34.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1672  -57.0000 -150.0000 60

  5 omega  -95.00    5.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1672  -77.0000  -30.0000 100
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0103687000
_diffrn_orient_matrix_UB_12      -0.0106114000
_diffrn_orient_matrix_UB_13      0.0447244000
_diffrn_orient_matrix_UB_21      0.0692620000
_diffrn_orient_matrix_UB_22      0.0199435000
_diffrn_orient_matrix_UB_23      0.0117974000
_diffrn_orient_matrix_UB_31      -0.0345851000
_diffrn_orient_matrix_UB_32      0.0366699000
_diffrn_orient_matrix_UB_33      0.0065454000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21490
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.17
_diffrn_reflns_theta_min         2.81
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    2.904
_exptl_absorpt_correction_T_max  0.568
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_recrystallization_method Benzene-d6
_exptl_crystal_size_max          0.2323
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.1604
_refine_diff_density_max         1.464
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.029(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         13229
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+1.3374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                12137
_reflns_number_total             13229
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401783c_si_001_1.cif
_cod_data_source_block           3c
_cod_original_cell_volume        2371.33(7)
_cod_database_code               4336814
_chemical_oxdiff_formula         'C50 H55 H4 P1 Ir1 B1 F4 O1'
_chemical_oxdiff_usercomment     'Marianna's Ir41'
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H6 of C6, H8 of C8, H17 of C17, H15 of C15, H3 of C3, H2 of C2, H50 of C50,
  H48 of C48, H51 of C51, H47 of C47, H52 of C52, H49 of C49, H30 of C30, H24
  of C24, H40 of C40, H31 of C31, H23 of C23, H26 of C26, H25 of C25, H27 of
  C27, H41 of C41, H32 of C32, H44 of C44, H39 of C39, H29 of C29, H38 of C38,
  H42 of C42, H37 of C37, H36 of C36, H35 of C35, H33 of C33, H43 of C43
 At 1.5 times of:
  {H20A,H20B,H20C} of C20, {H21A,H21B,H21C} of C21, {H19A,H19B,H19C} of C19,
  {H10A,H10B,H10C} of C10, {H11A,H11B,H11C} of C11, {H12A,H12B,H12C} of C12,
  {H46A,H46B,H46C} of C46
2. Restrained distances
 Ir1-H1A = Ir1-H1B
 1.603 with sigma of 0.002
 B1-F1 = B1-F2 = B1-F3 = B1-F4
 1.4 with sigma of 0.01
 B1-F1A = B1-F2A = B1-F3A = B1-F4A
 1.4 with sigma of 0.01
 F1A-F2A = F1A-F3A = F1A-F4A = F2A-F3A = F2A-F4A = F3A-F4A
 2.284 with sigma of 0.01
 F1-F2 = F1-F3 = F1-F4 = F2-F3 = F2-F4 = F3-F4
 2.284 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C46) ~ Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F1) = Uanis(F1A) = Uanis(F2) = Uanis(F2A) = Uanis(F3) = Uanis(F3A) 
= Uanis(F4) = Uanis(F4A)
4. others
 Sof(F1)=1-Sof(F1A)=Sof(F2)=1-Sof(F1A)=Sof(F3)=1-Sof(F1A)=Sof(F4)=1-Sof(F1A)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C15(H15), C17(H17), C23(H23), C24(H24),
 C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
  C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
 C42(H42), C43(H43), C44(H44), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51),
  C52(H52)
5.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C46(H46A,H46B,H46C)
;