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_7134740
_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 Ir8 O8 P16'
_chemical_formula_sum            'C300 H224 Cl8 Ir8 O8 P16'
_chemical_formula_weight         6273.50
_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 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_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                   11.573(2)
_cell_length_b                   22.229(4)
_cell_length_c                   46.579(10)
_cell_measurement_reflns_used    4612
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      21.628
_cell_measurement_theta_min      2.378
_cell_volume                     11983(4)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_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  0.0728
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            22455
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.793
_diffrn_reflns_theta_max         24.793
_diffrn_reflns_theta_min         2.030
_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    4.684
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0868 before and 0.0562 after correction.
The Ratio of minimum to maximum transmission is 0.8651.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear n/a yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   n/a
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       irregular
_exptl_crystal_F_000             6160
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.379
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         2588
_refine_ls_number_restraints     356
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+333.0524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1880
_reflns_number_total             2588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02201k2.cif
_cod_data_source_block           c1-ir
_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_sg_symbol_H-M      Fddd
_cod_database_code               7134740
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.706
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Ir1-P1A \\sim Ir1-P1
 with sigma of 0.02
 P1A-C3 \\sim P1-C3A \\sim P1A-C15 \\sim P1-C15A \\sim P1A-C9 \\sim P1-C9A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C16A) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C18A) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. 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) 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) P1A(0.5) C3A(0.5) C4A(0.5) H4A(0.5) C5A(0.5) H5A(0.5) C6A(0.5)
 C7A(0.5) H7A(0.5) C8A(0.5) H8A(0.5) C9A(0.5) C10A(0.5) H10A(0.5) C11A(0.5)
 H11A(0.5) C12A(0.5) H12A(0.5) C13A(0.5) H13A(0.5) C14A(0.5) H14A(0.5)
 C15A(0.5) C20A(0.5) H20A(0.5) C19A(0.5) H19A(0.5) C18A(0.5) H18A(0.5)
 C17A(0.5) H17A(0.5) C16A(0.5) H16A(0.5)
6.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), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C4A(H4A), C5A(H5A),
  C7A(H7A), C8A(H8A), C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A),
 C14A(H14A), C20A(H20A), C19A(H19A), C18A(H18A), C17A(H17A), C16A(H16A)
6.b Fitted hexagon refined as free rotating group:
 C3(C8,C7,C6,C5,C4), C9(C10,C11,C12,C13,C14), C15(C16,C17,C18,C19,C20),
 C3A(C4A,C5A,C6A,C7A,C8A), C9A(C10A,C11A,C12A,C13A,C14A), C15A(C20A,C19A,C18A,
 C17A,C16A)
;
_shelx_res_checksum              64503
_shelx_hkl_checksum              64003
_olex2_submission_special_instructions 'No special instructions were received'