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_4336815
_publ_contact_author_name
;
;
_publ_section_title
;
 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_formula_moiety         'B F4, C43 H63 Ir N4 P'
_chemical_formula_sum            'C43 H63 B F4 Ir N4 P'
_chemical_formula_weight         945.95
_chemical_name_systematic
;
 ? 
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_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-25
_audit_creation_method
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  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
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_cell_angle_alpha                72.929(4)
_cell_angle_beta                 74.479(3)
_cell_angle_gamma                67.697(4)
_cell_formula_units_Z            2
_cell_length_a                   11.3239(2)
_cell_length_b                   11.5474(6)
_cell_length_c                   19.0446(7)
_cell_measurement_reflns_used    8294
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      28.2581
_cell_measurement_theta_min      2.8639
_cell_volume                     2167.88(16)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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_computing_molecular_graphics
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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.
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_computing_publication_material
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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.
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_computing_structure_refinement
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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 0.9292
_diffrn_measured_fraction_theta_max 0.9292
_diffrn_measurement_details
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  1 omega  -68.00  -35.00   1.0000   43.4400
omega____ theta____ kappa____ phi______ frames
    -      -25.1392 -178.0000  -60.0000 33

  2 omega  -70.00    1.00   1.0000   43.4400
omega____ theta____ kappa____ phi______ frames
    -      -25.1392  -37.0000 -150.0000 71

  3 omega  -61.00  -35.00   1.0000   43.4400
omega____ theta____ kappa____ phi______ frames
    -      -25.1392 -178.0000    0.0000 26

  4 omega    5.00   17.00   1.0000   43.4400
omega____ theta____ kappa____ phi______ frames
    -       26.3892   77.0000 -150.0000 12

  5 omega   17.00   62.00   1.0000   43.4400
omega____ theta____ kappa____ phi______ frames
    -       26.3892  -99.0000  -60.0000 45

  6 omega   -1.00   89.00   1.0000   43.4400
omega____ theta____ kappa____ phi______ frames
    -       26.3892   77.0000  120.0000 90

  7 omega  -44.00   56.00   1.0000   43.4400
omega____ theta____ kappa____ phi______ frames
    -       26.3892  -77.0000    0.0000 100
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0184383000
_diffrn_orient_matrix_UB_12      -0.0677111000
_diffrn_orient_matrix_UB_13      0.0116004000
_diffrn_orient_matrix_UB_21      -0.0145339000
_diffrn_orient_matrix_UB_22      0.0052610000
_diffrn_orient_matrix_UB_23      0.0377777000
_diffrn_orient_matrix_UB_31      -0.0646521000
_diffrn_orient_matrix_UB_32      0.0031400000
_diffrn_orient_matrix_UB_33      0.0022524000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17060
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.87
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    3.168
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       plate
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.2223
_exptl_crystal_size_mid          0.0756
_exptl_crystal_size_min          0.0218
_refine_diff_density_max         3.007
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         10173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0233P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                9120
_reflns_number_total             10173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401783c_si_001_2.cif
_cod_data_source_block           5
_cod_original_cell_volume        2167.89(16)
_cod_database_code               4336815
_chemical_oxdiff_formula         'C43 H63 B1 F4 Ir1 N4 P1'
_chemical_oxdiff_usercomment     'Marianna IMesPCy3'
_reflns_odcompleteness_completeness 94.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.26
_olex2_refinement_description
;
;