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_7061677
_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         'C30 H66 O7 P2 Rh2 Si2'
_chemical_formula_sum            'C30 H66 O7 P2 Rh2 Si2'
_chemical_formula_weight         862.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-05-24 deposited with the CCDC.	2022-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.738(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3842(4)
_cell_length_b                   11.6384(2)
_cell_length_c                   17.9317(4)
_cell_measurement_reflns_used    36358
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5800
_cell_measurement_theta_min      2.2560
_cell_volume                     4028.63(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.908
_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    -88.00  80.00   0.50    0.80    --    1.10  28.00 -90.00  336
  2  \w      9.00  90.00   0.50    0.80    --    1.10  37.00  30.00  162
  3  \w    -84.00  -3.00   0.50    0.80    --    1.10  46.00   0.00  162
  4  \w    -72.00 -46.00   0.50    0.80    --    1.10  37.00  30.00   52
  5  \w    -58.00 -32.00   0.50    0.80    --   -1.40  46.00 -60.00   52
  6  \w     17.00  47.00   0.50    0.80    --   -1.40  46.00 -60.00   60
  7  \w    -91.00  88.00   0.50    0.80    --   -1.40  40.00 113.92  358
;
_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      0.0014842000
_diffrn_orient_matrix_UB_12      0.0484713000
_diffrn_orient_matrix_UB_13      0.0244939000
_diffrn_orient_matrix_UB_21      -0.0367265000
_diffrn_orient_matrix_UB_22      0.0020776000
_diffrn_orient_matrix_UB_23      -0.0125274000
_diffrn_orient_matrix_UB_31      -0.0000960000
_diffrn_orient_matrix_UB_32      -0.0368655000
_diffrn_orient_matrix_UB_33      0.0314252000
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            89146
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.471
_diffrn_reflns_theta_min         2.191
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       plate
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.287
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         10164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.003
_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          0.1032
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9113
_reflns_number_total             10164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03095k2.cif
_cod_data_source_block           ishi50p_auto
_cod_depositor_comments
'Adding full bibliography for 7061675--7061677.cif.'
_cod_database_code               7061677
_shelx_shelxl_version_number     2016/3
_chemical_oxdiff_formula         C30H66Si2O7P2Rh2
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C00E(H00E), C00H(H00H), C00I(H00I), C00O(H00O)
2.b Secondary CH2 refined with riding coordinates:
 C00M(H00J,H00K), C00N(H00L,H00M), C00R(H00U,H00V), C00X(H3,HH)
2.c Idealised Me refined as rotating group:
 C00J(H00A,H00B,H00C), C00K(H00D,H00F,H00G), C00P(H00N,H00P,H00Q), C00Q(H00R,
 H00S,H00T), C00S(H00W,H00X,H00Y), C00T(H00Z,H,HA), C00U(H00,HB,HC), C00V(H1,HD,
 HE), C00W(H2,HF,HG), C00Y(H4,HI,HJ), C00Z(H5,HK,HL), C011(H01A,H01B,H01C),
 C012(H01D,H01E,H01F), C013(H01G,H01H,H01I), C014(H01J,H01K,H01L), C015(H01M,
 H01N,H01O), C016(H01P,H01Q,H01R), C017(H01S,H01T,H01U)
;
_shelx_res_checksum              88479
_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 1.307
_oxdiff_exptl_absorpt_empirical_full_min 0.814