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_1564628
_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         'C25 H36 Cl2 N2 O5 Ru, 2(C H Cl3)'
_chemical_formula_sum            'C27 H38 Cl8 N2 O5 Ru'
_chemical_formula_weight         855.298
_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_Int_Tables_number      4
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 99.9494(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.86878(13)
_cell_length_b                   19.0328(4)
_cell_length_c                   12.1261(2)
_cell_measurement_reflns_used    6634
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      73.8410
_cell_measurement_theta_min      3.6780
_cell_volume                     1788.75(6)
_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      99.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.7110
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9928
_diffrn_measured_fraction_theta_max 0.9650
_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    -67.00  24.00   1.00    1.00    --  -40.55  57.00  30.00   91
  2  \w   -115.00 -24.00   1.00    1.00    --  -40.55 -38.00-120.00   91
  3  \w     34.00  81.00   1.00    1.77    --  106.89 -45.00 -60.00   47
  4  \w     80.00 156.00   1.00    1.77    --  106.89  30.00-150.00   76
  5  \w    107.00 158.00   1.00    1.77    --  106.89  15.00  90.00   51
  6  \w     85.00 130.00   1.00    1.77    --  106.89 -45.00 -60.00   45
  7  \w     85.00 140.00   1.00    1.77    --  106.89  45.00 150.00   55
  8  \w     34.00 121.00   1.00    1.77    --  106.89-125.00 -60.00   87
  9  \w    -69.00  33.00   1.00    1.00    --  -40.55  57.00-180.00  102
 10  \w      8.00 117.00   1.00    1.00    --   40.55  77.00  30.00  109
 11  \w     78.00 158.00   1.00    1.77    --  106.89  61.00 -60.00   80
 12  \w     35.00 112.00   1.00    1.77    --  106.89 -61.00  60.00   77
 13  \w     78.00 158.00   1.00    1.77    --  106.89  61.00   0.00   80
;
_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      0.1684744000
_diffrn_orient_matrix_UB_12      -0.0346601000
_diffrn_orient_matrix_UB_13      -0.0210317000
_diffrn_orient_matrix_UB_21      -0.0919962000
_diffrn_orient_matrix_UB_22      -0.0246845000
_diffrn_orient_matrix_UB_23      -0.1161134000
_diffrn_orient_matrix_UB_31      0.0518417000
_diffrn_orient_matrix_UB_32      0.0688432000
_diffrn_orient_matrix_UB_33      -0.0520437000
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.9928
_diffrn_reflns_Laue_measured_fraction_max 0.9650
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10401
_diffrn_reflns_point_group_measured_fraction_full 0.8561
_diffrn_reflns_point_group_measured_fraction_max 0.8167
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         73.90
_diffrn_reflns_theta_min         3.70
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.363
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.540
_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            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       block
_exptl_crystal_F_000             876.127
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.6152
_refine_diff_density_min         -0.6923
_refine_diff_density_rms         0.1110
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.016(12)
_refine_ls_d_res_high            0.8024
_refine_ls_d_res_low             11.9437
_refine_ls_goodness_of_fit_ref   1.0186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    59
_refine_ls_number_parameters     396
_refine_ls_number_reflns         5930
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0186
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.3628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0820
_reflns_Friedel_coverage         0.659
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              22
_reflns_limit_k_min              -19
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                5525
_reflns_number_total             5930
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ICA-2020-508-119651.cif
_cod_data_source_block           Crystal228
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               1564628
_chemical_oxdiff_formula         BiC26H45Cl2N3
_reflns_odcompleteness_completeness 99.43
_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 Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C1(H1), C5(H5), C4(H4), C1S(H1S), C2S(H2S)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C15(H15), C21(H21), C16(H16), C19(H19)
2.d Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C17(H17a,H17b,H17c), C25(H25a,H25b,H25c), C24(H24a,H24b,
 H24c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C26(H26a,H26b,
 H26c)
;