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_1564629
_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 N2 O5 Rh, 0.167(C H2 Cl2)'
_chemical_formula_sum            'C32.167 H43.333 Cl2.333 N2 O5 Rh'
_chemical_formula_weight         723.715
_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                79.890(3)
_cell_angle_beta                 81.498(3)
_cell_angle_gamma                89.261(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8667(3)
_cell_length_b                   10.9861(4)
_cell_length_c                   20.5635(6)
_cell_measurement_reflns_used    10508
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      74.0140
_cell_measurement_theta_min      4.0590
_cell_volume                     1730.21(11)
_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      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.7110
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9933
_diffrn_measured_fraction_theta_max 0.9655
_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   -117.00 -17.00   1.00    1.00    --  -40.55 -77.00 -60.00  100
  2  \w    -20.00  80.00   1.00    1.00    --   40.55 -99.00  60.00  100
  3  \w    -31.00  69.00   1.00    1.00    --   40.55 -57.00 150.00  100
  4  \w     42.00 131.00   1.00    2.48    --  106.89 -77.00 -30.00   89
  5  \w     35.00 135.00   1.00    2.48    --  106.89 -61.00  90.00  100
  6  \w     35.00 128.00   1.00    2.48    --  106.89 -45.00-150.00   93
  7  \w     54.00 158.00   1.00    2.48    --  106.89  15.00-180.00  104
  8  \w     34.00 121.00   1.00    2.48    --  106.89-125.00 -90.00   87
  9  \w     32.00  59.00   1.00    2.48    --  106.89 -94.00  90.00   27
 10  \w     77.00 105.00   1.00    2.48    --  106.89 -94.00  90.00   28
 11  \w     56.00 157.00   1.00    2.48    --  106.89  15.00  90.00  101
 12  \w   -113.00 -12.00   1.00    1.00    --  -40.55 -57.00-180.00  101
 13  \w     12.00 114.00   1.00    1.00    --   40.55  57.00  30.00  102
 14  \w      8.00 117.00   1.00    1.00    --   40.55  77.00  90.00  109
 15  \w     74.00 158.00   1.00    2.48    --  106.89  77.00-180.00   84
 16  \w     81.00 158.00   1.00    2.48    --  106.89  45.00 -30.00   77
 17  \w     74.00 158.00   1.00    2.48    --  106.89  77.00  30.00   84
 18  \w     78.00 158.00   1.00    2.48    --  106.89  61.00  90.00   80
 19  \w     74.00 158.00   1.00    2.48    --  106.89  77.00 -90.00   84
 20  \w     79.00 158.00   1.00    2.48    --  106.89  30.00 -90.00   79
 21  \w      8.00  94.00   1.00    1.00    --   40.55  77.00-180.00   86
 22  \w      2.00  97.00   1.00    1.00    --   40.55-125.00 -30.00   95
;
_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      -0.1049267000
_diffrn_orient_matrix_UB_12      -0.0906888000
_diffrn_orient_matrix_UB_13      -0.0281312000
_diffrn_orient_matrix_UB_21      -0.1358919000
_diffrn_orient_matrix_UB_22      0.1001034000
_diffrn_orient_matrix_UB_23      -0.0128609000
_diffrn_orient_matrix_UB_31      0.0986855000
_diffrn_orient_matrix_UB_32      0.0452528000
_diffrn_orient_matrix_UB_33      -0.0704538000
_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  0.0643
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.9933
_diffrn_reflns_Laue_measured_fraction_max 0.9655
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19292
_diffrn_reflns_point_group_measured_fraction_full 0.8488
_diffrn_reflns_point_group_measured_fraction_max 0.8126
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         73.93
_diffrn_reflns_theta_min         4.09
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.971
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.837
_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    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             754.164
_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.1013
_refine_diff_density_min         -1.3635
_refine_diff_density_rms         0.1466
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.009(12)
_refine_ls_d_res_high            0.8023
_refine_ls_d_res_low             10.8145
_refine_ls_goodness_of_fit_ref   1.0408
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    134
_refine_ls_number_parameters     784
_refine_ls_number_reflns         11414
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0408
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1224P)^2^+5.3379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1916
_reflns_Friedel_coverage         0.660
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              25
_reflns_limit_l_min              -25
_reflns_number_gt                10142
_reflns_number_total             11414
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ICA-2020-508-119651.cif
_cod_data_source_block           Crystal271
_cod_original_cell_volume        1730.2(1)
_cod_original_sg_symbol_Hall     ' P 1'
_cod_database_code               1564629
_chemical_oxdiff_formula         RhCl2N2C36H45O6
_reflns_odcompleteness_completeness 99.35
_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. Others
 Fixed Sof: Cl1S(0.33333) Cl2S(0.33333) C1S(0.33333) H1Sa(0.33333) H1Sb(0.33333)
3.a Riding coordinates:
 C30B(H30d,H30e,H30f,C25B), C9A(C7A,H21A,H9Aa,H9Ab,H9Ac)
3.b Ternary CH refined with riding coordinates:
 C3B(H3B), C3A(H3A), C2B(H2B), C4A(H4A), C2A(H2A), C1B(H1B), C5B(H5B),
 C5A(H5A), C4B(H4B), C1A(H1A)
3.c Secondary CH2 refined with riding coordinates:
 C16A(H16a,H16b), C16B(H16c,H16d), C6B(H6Ba,H6Bb), C6A(H6Aa,H6Ab), C1S(H1Sa,
 H1Sb)
3.d Aromatic/amide H refined with riding coordinates:
 C14B(H14B), C14A(H14A), C15B(H15B), C15A(H15A), C18A(H18A), C22B(H22B),
 C18B(H18B), C19B(H19B), C22A(H22A), C21B(H21B), C19A(H19A), C20B(H20B),
 C20A(H20A)
3.e Idealised Me refined as rotating group:
 C28B(H28d,H28e,H28f), C29B(H29d,H29e,H29f), C28A(H28a,H28b,H28c), C29A(H29a,
 H29b,H29c), C30A(H30a,H30b,H30c), C31A(H31a,H31b,H31c), C12B(H12d,H12e,H12f),
 C32A(H32a,H32b,H32c), C31B(H31d,H31e,H31f), C9B(H9Ba,H9Bb,H9Bc), C32B(H32d,
 H32e,H32f), C8B(H8Ba,H8Bb,H8Bc), C11B(H11d,H11e,H11f), C12A(H12a,H12b,H12c),
 C11A(H11a,H11b,H11c), C8A(H8Aa,H8Ab,H8Ac)
;