Piano stool complexes of N-heterocyclic carbene ligands bearing a galactose-derived substituent
Bandaru, Sravan K.; Thomas, Hayden P.; Saunders, Graham C.; Inorganica Chimica Acta 508 (2020) 119651–; doi:10.1016/j.ica.2020.119651

data_1564627
_publ_section_title
;
 Piano stool complexes of N-heterocyclic carbene ligands bearing a
 galactose-derived substituent
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119651
_journal_paper_doi               10.1016/j.ica.2020.119651
_journal_volume                  508
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C32 H43 Cl2 Ir N2 O5'
_chemical_formula_sum            'C32 H43 Cl2 Ir N2 O5'
_chemical_formula_weight         798.830
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_Int_Tables_number      1
_atom_sites_solution_primary     iterative
_cell_angle_alpha                80.0645(14)
_cell_angle_beta                 81.6655(16)
_cell_angle_gamma                89.1459(14)
_cell_formula_units_Z            2
_cell_length_a                   7.85321(15)
_cell_length_b                   10.98822(16)
_cell_length_c                   20.4662(4)
_cell_measurement_reflns_used    34763
_cell_measurement_temperature    99.96(17)
_cell_measurement_theta_max      73.9870
_cell_measurement_theta_min      4.0500
_cell_volume                     1721.13(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.96(17)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.7110
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9911
_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     -2.00  25.00   1.00    1.00    --   36.00  93.00 101.52   27
  2  \w    -51.00 -12.00   1.00    1.00    --  -40.55 -57.00   0.00   39
  3  \w   -108.00 -66.00   1.00    1.00    --  -40.55 -57.00   0.00   42
  4  \w    -91.00 -37.00   1.00    1.00    --  -40.55 125.00 -60.00   54
  5  \w   -113.00 -15.00   1.00    1.00    --  -40.55 -57.00 -90.00   98
  6  \w    -64.00  34.00   1.00    1.00    --  -40.55  38.00  60.00   98
  7  \w     27.00 111.00   1.00    1.00    --   40.55  38.00  60.00   84
  8  \w     10.00  86.00   1.00    1.00    --   40.55-125.00-120.00   76
  9  \w      7.00  32.00   1.00    1.00    --   44.00  89.00 161.55   25
 10  \w     14.00  39.00   1.00    1.00    --   48.00  83.00 -15.69   25
 11  \w     14.00  39.00   1.00    1.00    --   48.00  81.00-143.87   25
 12  \w     19.00  44.00   1.00    1.00    --   52.00  80.00 -48.69   25
 13  \w     18.00  43.00   1.00    1.00    --   52.00  82.00  26.97   25
 14  \w     18.00  43.00   1.00    1.00    --   52.00  81.00  67.59   25
 15  \w     23.00  48.00   1.00    1.00    --   56.00  78.00-105.73   25
 16  \w     23.00  48.00   1.00    1.00    --   56.00  78.00 110.06   25
 17  \w     29.00  55.00   1.00    1.00    --   60.00  76.00 123.08   26
 18  \w     32.00  58.00   1.00    1.00    --   64.00  75.00 142.17   26
 19  \w     32.00  59.00   1.00    1.00    --   64.00  76.00 168.29   27
 20  \w     36.00  62.00   1.00    1.00    --   68.00  75.00-153.75   26
 21  \w     36.00  62.00   1.00    1.00    --   68.00  74.00 -51.31   26
 22  \w     76.00 141.00   1.00    1.00    --   68.00  69.00  75.45   65
 23  \w     37.00  65.00   1.00    1.00    --   68.00  69.00  75.45   28
 24  \w     44.00  69.00   1.00    1.00    --   72.00  59.00-168.81   25
 25  \w     41.00  88.00   1.00    1.00    --   72.00  74.00 -21.21   47
 26  \w     39.00  65.00   1.00    1.00    --   72.00  77.00  10.02   26
 27  \w     48.00  81.00   1.00    1.00    --   80.00  75.00-107.49   33
 28  \w     97.00 155.00   1.00    1.00    --   80.00  75.00-107.49   58
 29  \w     49.00  78.00   1.00    1.00    --   80.00  72.00-148.89   29
 30  \w    117.00 158.00   1.00    1.00    --  100.00  74.00   0.07   41
 31  \w     69.00  94.00   1.00    1.00    --  100.00  74.00   0.07   25
 32  \w     74.00 100.00   1.00    1.00    --  106.89  77.00 -90.00   26
 33  \w     74.00 152.00   1.00    1.00    --  106.89  77.00-180.00   78
 34  \w     82.00 115.00   1.00    1.00    --  106.89  61.00 120.00   33
 35  \w     78.00 116.00   1.00    1.00    --  106.89  61.00 -60.00   38
 36  \w     80.00 121.00   1.00    1.00    --  106.89-125.00-120.00   41
 37  \w     80.00 107.00   1.00    1.00    --  106.89  61.00  60.00   27
 38  \w     45.00  71.00   1.00    1.00    --  106.89-125.00-120.00   26
 39  \w     92.00 148.00   1.00    1.00    --  106.89 125.00 120.00   56
 40  \w     78.00 110.00   1.00    1.00    --  106.89  61.00  30.00   32
 41  \w     75.00 146.00   1.00    1.00    --  106.89  77.00-120.00   71
 42  \w     75.00 157.00   1.00    1.00    --  106.89  77.00 -60.00   82
 43  \w     74.00 157.00   1.00    1.00    --  106.89  77.00 120.00   83
 44  \w     74.00 111.00   1.00    1.00    --  106.89  77.00 150.00   37
 45  \w     74.00 101.00   1.00    1.00    --  106.89  77.00  60.00   27
 46  \w     31.00 129.00   1.00    1.00    --  106.89 -77.00  30.00   98
 47  \w    120.00 158.00   1.00    1.00    --  106.89  77.00-150.00   38
 48  \w     74.00 117.00   1.00    1.00    --  106.89  77.00-150.00   43
 49  \w     85.00 154.00   1.00    1.00    --  106.89  61.00  90.00   69
 50  \w     76.00 105.00   1.00    1.00    --  106.89-125.00 -30.00   29
 51  \w     35.00  60.00   1.00    1.00    --  106.89-125.00 -30.00   25
 52  \w     74.00 148.00   1.00    1.00    --  106.89  77.00 -30.00   74
 53  \w     74.00 100.00   1.00    1.00    --  106.89  77.00  90.00   26
 54  \w     75.00 122.00   1.00    1.00    --  106.89 -45.00  30.00   47
 55  \w     45.00  71.00   1.00    1.00    --  106.89 -45.00  30.00   26
 56  \w    110.00 156.00   1.00    1.00    --  106.89  77.00  30.00   46
 57  \w     35.00 136.00   1.00    1.00    --  106.89 -61.00 150.00  101
 58  \w     74.00 100.00   1.00    1.00    --  106.89  77.00  30.00   26
 59  \w     24.00 107.00   1.00    1.00    --  106.89 -94.00 -30.00   83
 60  \w    126.00 153.00   1.00    1.00    --  106.89  77.00 -90.00   27
 61  \w      3.00  33.00   1.00    1.00    --   40.00  89.00 110.84   30
 62  \w    -65.00  34.00   1.00    1.00    --  -40.55  38.00 -60.00   99
 63  \w    -20.00  81.00   1.00    1.00    --   40.55 -99.00  90.00  101
 64  \w      8.00  34.00   1.00    1.00    --   44.00  87.00 -38.72   26
 65  \w      8.00  34.00   1.00    1.00    --   44.00  87.00  -8.34   26
 66  \w     14.00  46.00   1.00    1.00    --   48.00  81.00-143.87   32
 67  \w     19.00  46.00   1.00    1.00    --   52.00  80.00-166.08   27
 68  \w     23.00  49.00   1.00    1.00    --   56.00  78.00  63.77   26
 69  \w     32.00 139.00   1.00    1.00    --   64.00  75.00 142.17  107
 70  \w     35.00 137.00   1.00    1.00    --   64.00  60.00 105.74  102
 71  \w     37.00 142.00   1.00    1.00    --   68.00  72.00-122.62  105
 72  \w     35.00 144.00   1.00    1.00    --   68.00  77.00-149.26  109
 73  \w     36.00 143.00   1.00    1.00    --   68.00  74.00 -51.31  107
 74  \w     43.00 145.00   1.00    1.00    --   72.00  59.00-168.81  102
 75  \w     40.00 147.00   1.00    1.00    --   72.00  74.00 -21.21  107
 76  \w     39.00 148.00   1.00    1.00    --   72.00  77.00  10.02  109
 77  \w     52.00 152.00   1.00    1.00    --   80.00  55.00-152.89  100
 78  \w     68.00 158.00   1.00    1.00    --  100.00  74.00   0.07   90
 79  \w     74.00 158.00   1.00    1.00    --  106.89  77.00  60.00   84
 80  \w     74.00 158.00   1.00    1.00    --  106.89  77.00   0.00   84
 81  \w     78.00 158.00   1.00    1.00    --  106.89  61.00-150.00   80
 82  \w     78.00 158.00   1.00    1.00    --  106.89  61.00 -90.00   80
 83  \w     78.00 158.00   1.00    1.00    --  106.89  61.00 150.00   80
 84  \w     73.00 158.00   1.00    1.00    --  106.89 125.00   0.00   85
 85  \w     34.00 121.00   1.00    1.00    --  106.89-125.00  90.00   87
 86  \w     78.00 158.00   1.00    1.00    --  106.89  61.00 -60.00   80
 87  \w     74.00 158.00   1.00    1.00    --  106.89  77.00 -30.00   84
 88  \w     81.00 158.00   1.00    1.00    --  106.89  45.00 120.00   77
 89  \w     78.00 158.00   1.00    1.00    --  106.89  61.00-120.00   80
 90  \w     31.00 139.00   1.00    1.00    --  106.89 -77.00   0.00  108
 91  \w     24.00 109.00   1.00    1.00    --  106.89 -94.00 150.00   85
 92  \w     81.00 158.00   1.00    1.00    --  106.89  45.00 150.00   77
 93  \w     73.00 158.00   1.00    1.00    --  106.89 125.00  30.00   85
 94  \w     78.00 158.00   1.00    1.00    --  106.89  61.00-180.00   80
 95  \w     24.00 109.00   1.00    1.00    --  106.89 -94.00 -30.00   85
 96  \w     74.00 158.00   1.00    1.00    --  106.89  77.00  30.00   84
 97  \w     31.00 139.00   1.00    1.00    --  106.89 -77.00-180.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0866574000
_diffrn_orient_matrix_UB_12      -0.1131696000
_diffrn_orient_matrix_UB_13      -0.0253347000
_diffrn_orient_matrix_UB_21      -0.1574732000
_diffrn_orient_matrix_UB_22      -0.0805941000
_diffrn_orient_matrix_UB_23      0.0343315000
_diffrn_orient_matrix_UB_31      -0.0836981000
_diffrn_orient_matrix_UB_32      0.0309663000
_diffrn_orient_matrix_UB_33      -0.0643747000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.9997
_diffrn_reflns_Laue_measured_fraction_max 0.9911
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59805
_diffrn_reflns_point_group_measured_fraction_full 0.9570
_diffrn_reflns_point_group_measured_fraction_max 0.9361
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         74.07
_diffrn_reflns_theta_min         4.08
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.256
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.541
_exptl_crystal_description       block
_exptl_crystal_F_000             795.083
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.042
_refine_diff_density_max         3.1188
_refine_diff_density_min         -2.8515
_refine_diff_density_rms         0.3081
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.011(14)
_refine_ls_d_res_high            0.8017
_refine_ls_d_res_low             10.8228
_refine_ls_goodness_of_fit_ref   1.0465
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    132
_refine_ls_number_parameters     724
_refine_ls_number_reflns         13100
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0465
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1215P)^2^+44.9237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.2062
_reflns_Friedel_coverage         0.881
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              24
_reflns_limit_l_min              -25
_reflns_number_gt                12239
_reflns_number_total             13100
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ICA-2020-508-119651.cif
_cod_data_source_block           Crystal287
_cod_original_sg_symbol_Hall     ' P 1'
_cod_database_code               1564627
_chemical_oxdiff_formula         IrCl2N2O10C37H46
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Riding coordinates:
 C3A(C29B,H29a,H29b,H29c,C24B), C12B(H12a,H12b,H12c,C10B)
2.b Ternary CH refined with riding coordinates:
 C3A(H3A), C3B(H3B), C5B(H5B), C2A(H2A), C1B(H1B), C2B(H2B), C4B(H4B),
 C4A(H4A), C1A(H1A), C5A(H5A)
2.c Secondary CH2 refined with riding coordinates:
 C16A(H16c,H16d), C16B(H16a,H16b), C6B(H6Ba,H6Bb), C6A(H6Aa,H6Ab)
2.d Aromatic/amide H refined with riding coordinates:
 C21A(H21A), C21B(H21B), C14A(H14A), C14B(H14B), C22B(H22B), C18A(H18A),
 C18B(H18B), C22A(H22A), C15A(H15A), C19B(H19B), C19A(H19A), C20B(H20B),
 C20A(H20A), C15B(H15B)
2.e Idealised Me refined as rotating group:
 C28A(H28d,H28e,H28f), C32A(H32d,H32e,H32f), C28B(H28a,H28b,H28c), C30B(H30a,
 H30b,H30c), C31A(H31d,H31e,H31f), C8B(H8Ba,H8Bb,H8Bc), C30A(H30d,H30e,H30f),
 C31B(H31a,H31b,H31c), C9B(H9Ba,H9Bb,H9Bc), C9A(H9Aa,H9Ab,H9Ac), C29A(H29d,H29e,
 H29f), C11B(H11a,H11b,H11c), C12A(H12d,H12e,H12f), C8A(H8Aa,H8Ab,H8Ac),
 C11A(H11d,H11e,H11f), C32B(H32a,H32b,H32c)
;