Exohedral functionalization vs. core expansion of siliconoids with Group 9 metals: catalytic activity in alkene isomerization
Poitiers, Nadine Elisabeth; Giarrana, Luisa; Huch, Volker; Zimmer, Michael; Scheschkewitz, David; Chemical Science  (2020) –; doi:10.1039/D0SC02861D

data_1558484
_publ_section_title
;
 Exohedral functionalization vs. core expansion of siliconoids with Group
 9 metals: catalytic activity in alkene isomerization
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02861D
_journal_year                    2020
_chemical_formula_moiety         'C92 H138 Cl N2 O2 Rh Si7'
_chemical_formula_sum            'C92 H138 Cl N2 O2 Rh Si7'
_chemical_formula_weight         1639.03
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-05-04 deposited with the CCDC.	2020-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.608(4)
_cell_length_b                   13.6961(14)
_cell_length_c                   18.1426(19)
_cell_measurement_reflns_used    3048
_cell_measurement_temperature    142(2)
_cell_measurement_theta_max      18.68
_cell_measurement_theta_min      2.44
_cell_volume                     9344.9(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      142(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            85115
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.934
_diffrn_reflns_theta_min         1.560
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             3520
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
; 
 Flack x determined using 7316 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.015(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1034
_refine_ls_number_reflns         22265
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0372P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                18546
_reflns_number_total             22265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02861d2.cif
_cod_data_source_block           sh3959
_cod_original_cell_volume        9345.0(17)
_cod_database_code               1558484
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              46654