Selective hydrosilylation of olefins by a two-dimensional Rh(I) low-valent metal-organic framework.
Mandal, Dipendu; Esposito, Madison R.; Griffin, Samuel E.; Domecus, Grant P.; Cohen, Seth M.; Chemical communications (Cambridge, England) 61 (2025) 10526–10529; doi:10.1039/d5cc02201k

data_7134739
_publ_section_title
;
 Selective hydrosilylation of olefins by a two-dimensional Rh(I)
 low-valent metal-organic framework.
;
_journal_issue                   57
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10526
_journal_page_last               10529
_journal_paper_doi               10.1039/d5cc02201k
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C300 H224 Cl8 O8 P16 Rh8'
_chemical_formula_sum            'C300 H224 Cl8 O8 P16 Rh8'
_chemical_formula_weight         5559.18
_chemical_name_systematic        C1-Rh
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-06-12 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6257(6)
_cell_length_b                   22.2356(13)
_cell_length_c                   46.905(3)
_cell_measurement_reflns_used    2494
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      23.77
_cell_measurement_theta_min      2.94
_cell_volume                     12125.1(12)
_computing_cell_refinement       'SAINT v8.40B (Bruker, 2019)'
_computing_data_collection       'APEX5 v2023.9-2 (Bruker, 2023)'
_computing_data_reduction        'SAINT v8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            13932
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         1.737
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_T_max  0.4903
_exptl_absorpt_correction_T_min  0.4226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1314 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.8619.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5648
_exptl_crystal_size_max          0.033
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.852
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         2773
_refine_ls_number_restraints     362
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1194P)^2^+129.7599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1944
_refine_ls_wR_factor_ref         0.2129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2110
_reflns_number_total             2773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02201k2.cif
_cod_data_source_block           c1-rh
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7134739--7134740.cif.
;
_cod_original_cell_volume        12125.0(12)
_cod_original_sg_symbol_H-M      Fddd
_cod_database_code               7134739
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.974
_olex2_refinement_description
;
1. Restrained distances
 Rh1-P1 \\sim Rh1-P1'
 with sigma of 0.02
 P1'-C15' \\sim P1-C15 \\sim P1'-C9' \\sim P1-C9 \\sim P1'-C3' \\sim P1-C3
 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19')
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: Cl1(0.5) P1'(0.5) C3'(0.5) C8'(0.5) H8'(0.5) C7'(0.5) H7'(0.5)
 C6'(0.5) C5'(0.5) H5'(0.5) C4'(0.5) H4'(0.5) C9'(0.5) C10'(0.5) H10'(0.5)
 C11'(0.5) H11'(0.5) C12'(0.5) H12'(0.5) C13'(0.5) H13'(0.5) C14'(0.5)
 H14'(0.5) C15'(0.5) C20'(0.5) H20'(0.5) C19'(0.5) H19'(0.5) C18'(0.5)
 H18'(0.5) C17'(0.5) H17'(0.5) C16'(0.5) H16'(0.5) P1(0.5) C3(0.5) C4(0.5)
 H4(0.5) C5(0.5) H5(0.5) C6(0.5) C7(0.5) H7(0.5) C8(0.5) H8(0.5) C9(0.5)
 C14(0.5) H14(0.5) C13(0.5) H13(0.5) C12(0.5) H12(0.5) C11(0.5) H11(0.5)
 C10(0.5) H10(0.5) C15(0.5) C16(0.5) H16(0.5) C17(0.5) H17(0.5) C18(0.5)
 H18(0.5) C19(0.5) H19(0.5) C20(0.5) H20(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C8'(H8'), C7'(H7'), C5'(H5'), C4'(H4'), C10'(H10'), C11'(H11'), C12'(H12'),
 C13'(H13'), C14'(H14'), C20'(H20'), C19'(H19'), C18'(H18'), C17'(H17'),
 C16'(H16'), C4(H4), C5(H5), C7(H7), C8(H8), C14(H14), C13(H13), C12(H12),
 C11(H11), C10(H10), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
5.b Fitted hexagon refined as free rotating group:
 C3'(C8',C7',C6',C5',C4'), C9'(C10',C11',C12',C13',C14'), C15'(C20',C19',C18',
 C17',C16'), C3(C4,C5,C6,C7,C8), C9(C14,C13,C12,C11,C10), C15(C16,C17,C18,C19,
 C20)
;
_shelx_res_checksum              21181
_shelx_hkl_checksum              72881
_olex2_submission_special_instructions 'No special instructions were received'