Ir-Catalyzed Selective Reduction of CO2 to Methoxy or Formate Level with HSiMe(OSiMe3)2
Guzman, Jefferson; García-Orduña, Pilar; Polo, Victor; Lahoz, Fernando J.; Oro, Luis A.; Fernandez-Alvarez, Francisco J; Catalysis Science & Technology  (2019) –; doi:10.1039/C8CY02353K

data_1550935
_publ_section_title
;
 Ir-Catalyzed Selective Reduction of CO2 to Methoxy or Formate Level with
 HSiMe(OSiMe3)2
;
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_paper_doi               10.1039/C8CY02353K
_journal_year                    2019
_chemical_formula_moiety         '2(C18 H24 F3 Ir N2 O4 Si2), 0.5(C4 H10 O)'
_chemical_formula_sum            'C38 H53 F6 Ir2 N4 O8.5 Si4'
_chemical_formula_weight         1312.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-07-26 deposited with the CCDC.    2019-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.2260(10)
_cell_angle_beta                 106.8990(10)
_cell_angle_gamma                101.8860(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4358(6)
_cell_length_b                   13.0237(7)
_cell_length_c                   17.6415(9)
_cell_measurement_reflns_used    9588
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2875
_cell_measurement_theta_min      2.202
_cell_volume                     2454.4(2)
_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-2017/1 (Sheldrick, 2017)'
_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 0.967
_diffrn_measurement_device_type  'Bruker Smart APEX 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  0.0292
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47378
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.430
_diffrn_reflns_theta_min         1.906
_exptl_absorpt_coefficient_mu    5.588
_exptl_absorpt_correction_T_max  0.5633
_exptl_absorpt_correction_T_min  0.4502
_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            yellow
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       prism
_exptl_crystal_F_000             1282
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.125
_refine_diff_density_max         1.272
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         11954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0272P)^2^+4.0995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0625
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10240
_reflns_number_total             11954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cy02353k2.cif
_cod_data_source_block           cmpnd_3
_cod_original_formula_sum        'C38 H53 F6 Ir2 N4 O8.50 Si4'
_cod_database_code               1550935
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              80061