Multinuclear rhodium complexes supported by tetra-tert-butoxy disiloxide ligand: synthesis, structure, and reactivity
Ishizaka, Yusuke; Matsumoto, Kazuhiro; Sato, Kazuhiko; Choi, Jun-Chul; New Journal of Chemistry 46 (2022) 16040–16046; doi:10.1039/D2NJ03095K

data_7061675
_publ_section_title
;
 Multinuclear rhodium complexes supported by tetra-tert-butoxy disiloxide
 ligand: synthesis, structure, and reactivity
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16040
_journal_page_last               16046
_journal_paper_doi               10.1039/D2NJ03095K
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C20 H36 O11 Rh2 Si2'
_chemical_formula_sum            'C20 H36 O11 Rh2 Si2'
_chemical_formula_weight         714.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-05-24 deposited with the CCDC.	2022-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                112.248(2)
_cell_angle_beta                 99.310(2)
_cell_angle_gamma                99.762(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3394(2)
_cell_length_b                   11.5662(2)
_cell_length_c                   14.9335(3)
_cell_measurement_reflns_used    15798
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.3300
_cell_measurement_theta_min      2.8330
_cell_volume                     1425.56(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.881
_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     62.00  93.00   0.50   17.58    --    5.00  31.00 -64.35   62
  2  \w    -84.00  -2.00   0.50   17.58    --    5.00  31.00 -64.35  164
  3  \w    -87.00 -59.00   0.50   17.58    --   -8.00  28.00 120.00   56
  4  \w    -97.00 -69.00   0.50   17.58    --   -8.00  55.00-150.00   56
  5  \w    -35.00  81.00   0.50   17.58    --   -8.00  55.00-150.00  232
  6  \w    -35.00  70.00   0.50   17.58    --   -8.00  46.00  60.00  210
  7  \w    -12.00  28.00   0.50   17.58    --   -8.00  18.00-150.00   80
  8  \w    -87.00 -28.00   0.50   17.58    --   -8.00  18.00-150.00  118
  9  \w     38.00  78.00   0.50   17.58    --   -8.00  18.00-150.00   80
 10  \w    -34.00  50.00   0.50   17.58    --   -8.00  28.00 120.00  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0690610000
_diffrn_orient_matrix_UB_12      -0.0361397000
_diffrn_orient_matrix_UB_13      0.0004785000
_diffrn_orient_matrix_UB_21      0.0035273000
_diffrn_orient_matrix_UB_22      0.0480466000
_diffrn_orient_matrix_UB_23      0.0476552000
_diffrn_orient_matrix_UB_31      -0.0393091000
_diffrn_orient_matrix_UB_32      0.0327867000
_diffrn_orient_matrix_UB_33      -0.0231178000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27825
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.164
_diffrn_reflns_theta_min         2.284
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       plate
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.290
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.768
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         7440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.768
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6392
_reflns_number_total             7440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03095k2.cif
_cod_data_source_block           ishi33p
_cod_depositor_comments
'Adding full bibliography for 7061675--7061677.cif.'
_cod_original_cell_volume        1425.56(5)
_cod_database_code               7061675
_shelx_shelxl_version_number     2016/3
_chemical_oxdiff_formula         C20H36O11Si2Rh
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.893
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C00G(H00A,H00B,H00C), C00J(H00D,H00E,H00F), C00L(H00G,H00H,H00I), C00O(H00J,
 H00K,H00L), C00P(H00M,H00N,H00O), C00S(H00P,H00Q,H00R), C00T(H00S,H00T,H00U),
 C00V(H00V,H00W,H00X), C00W(H00Y,H,HA), C00X(H00Z,HB,HC), C00Y(H00,HD,HE),
 C00Z(H1,HF,HG)
;
_shelx_res_checksum              12364
_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 1.701
_oxdiff_exptl_absorpt_empirical_full_min 0.820