Iridium Cyclooctene Complex That Forms a Hyperpolarization Transfer Catalyst before Converting to a Binuclear C-H Bond Activation Product Responsible for Hydrogen Isotope Exchange.
Iali, Wissam; Green, Gary G. R.; Hart, Sam J.; Whitwood, Adrian C.; Duckett, Simon B.; Inorganic chemistry 55 (2016) 11639–11643; doi:10.1021/acs.inorgchem.6b02560

data_4349348
_publ_section_title
;
 Iridium Cyclooctene Complex That Forms a Hyperpolarization Transfer
 Catalyst before Converting to a Binuclear C-H Bond Activation Product
 Responsible for Hydrogen Isotope Exchange.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11639
_journal_page_last               11643
_journal_paper_doi               10.1021/acs.inorgchem.6b02560
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C20 H22 Cl2 Ir2 N4, C4 H8 O'
_chemical_formula_sum            'C24 H30 Cl2 Ir2 N4 O'
_chemical_formula_weight         845.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2950(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.33293(13)
_cell_length_b                   13.35619(19)
_cell_length_c                   18.9458(2)
_cell_measurement_reflns_used    19625
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      32.0570
_cell_measurement_theta_min      3.5780
_cell_volume                     2598.92(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     -5.00  96.00   1.00    5.00    --   25.48  77.00  60.00  101
  2  \w      5.00  94.00   1.00    5.00    --   25.48  57.00 -60.00   89
  3  \w    -20.00  67.00   1.00    5.00    --   25.48 -99.00 120.00   87
  4  \w      0.00  98.00   1.00    5.00    --   25.48  37.00 -30.00   98
  5  \w    -45.00  56.00   1.00    5.00    --   25.48 -77.00-180.00  101
  6  \w      0.00  98.00   1.00    5.00    --   25.48  37.00-150.00   98
  7  \w     35.00  63.00   1.00    5.00    --   25.48 178.00  30.00   28
  8  \w   -102.00 -57.00   1.00    5.00    --  -26.10-178.00-120.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0279619000
_diffrn_orient_matrix_UB_12      0.0222008000
_diffrn_orient_matrix_UB_13      0.0321184000
_diffrn_orient_matrix_UB_21      0.0609138000
_diffrn_orient_matrix_UB_22      0.0028731000
_diffrn_orient_matrix_UB_23      -0.0138646000
_diffrn_orient_matrix_UB_31      -0.0165045000
_diffrn_orient_matrix_UB_32      0.0481874000
_diffrn_orient_matrix_UB_33      -0.0139527000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40460
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         32.170
_diffrn_reflns_theta_min         3.447
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.460
_exptl_absorpt_correction_T_max  0.166
_exptl_absorpt_correction_T_min  0.068
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.162
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_recrystallization_method THF
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.285
_refine_diff_density_max         2.604
_refine_diff_density_min         -3.144
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         8539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+1.7599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7725
_reflns_number_total             8539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02560_si_003.cif
_cod_data_source_block           complex_4
_cod_original_cell_volume        2598.91(6)
_cod_database_code               4349348
_chemical_oxdiff_formula         'C24 H30 Cl2 Ir2 N4 O'
_chemical_oxdiff_usercomment     'Wissam Iali IrPyridol'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Riding coordinates:
 Ir2(HB)
2.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
  C19(H19), C20(H20)
;
_shelx_res_checksum              78883
_shelx_hkl_checksum              43608
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-02-02
_olex2_date_sample_submission    2016-01-25
_olex2_exptl_crystal_mounting_method 'oil on micromount'
_olex2_submission_original_sample_id IrPyridol
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.893
_oxdiff_exptl_absorpt_empirical_full_min 0.653