Unprecedent formation of methylsilylcarbonates from iridium-catalyzed reduction of CO2 with hydrosilanes
Guzmán, Jefferson; García-Orduña, Pilar; Lahoz, Fernando J.; Fernández-Alvarez, Francisco J.; RSC Advances 10 (2020) 9582–9586; doi:10.1039/D0RA00204F

data_7240092
_publ_section_title
;
 Unprecedent formation of methylsilylcarbonates from iridium-catalyzed
 reduction of CO2 with hydrosilanes
;
_journal_issue                   16
_journal_name_full               'RSC Advances'
_journal_page_first              9582
_journal_page_last               9586
_journal_paper_doi               10.1039/D0RA00204F
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C34 H48 F6 Ir2 N4 O10 S2 Si4, 0.5(H2 O)'
_chemical_formula_sum            'C34 H49 F6 Ir2 N4 O10.5 S2 Si4'
_chemical_formula_weight         1364.65
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-12-16 deposited with the CCDC.	2020-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                66.4720(10)
_cell_angle_beta                 88.5460(10)
_cell_angle_gamma                88.7690(10)
_cell_formula_units_Z            1
_cell_length_a                   9.0468(5)
_cell_length_b                   12.0453(6)
_cell_length_c                   12.0619(7)
_cell_measurement_reflns_used    9787
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.366
_cell_measurement_theta_min      2.252
_cell_volume                     1204.65(11)
_computing_cell_refinement
'SAINT+ in APEX3 v. 2017.3 (Bruker AXS, 2008)'
_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction
'SAINT+ in APEX3 v. 2017.3 (Bruker AXS, 2008)'
_computing_molecular_graphics    'ORTEP-3 (farrugia, 2012)'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX CCD system'
_diffrn_measurement_method       'narrow \w frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23425
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.389
_diffrn_reflns_theta_min         2.021
_exptl_absorpt_coefficient_mu    5.783
_exptl_absorpt_correction_T_max  0.5996
_exptl_absorpt_correction_T_min  0.1676
_exptl_absorpt_correction_type   numerical
_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            colourless
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_description       prism
_exptl_crystal_F_000             665
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0134
_refine_ls_R_factor_gt           0.0131
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0134P)^2^+0.9702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0323
_refine_ls_wR_factor_ref         0.0324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5771
_reflns_number_total             5849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra00204f2.cif
_cod_data_source_block           cmpnd_3
_cod_depositor_comments          'Adding full bibliography for 7240092.cif.'
_cod_original_formula_sum        'C34 H49 F6 Ir2 N4 O10.50 S2 Si4'
_cod_database_code               7240092
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              53737
_shelx_fab_checksum              58770