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_1550934
_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         'C32 H48 Cl2 Ir2 N4 O4 Si4'
_chemical_formula_sum            'C32 H48 Cl2 Ir2 N4 O4 Si4'
_chemical_formula_weight         1120.40
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-07-26 deposited with the CCDC.    2019-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.227(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8492(9)
_cell_length_b                   10.6328(6)
_cell_length_c                   43.5137(19)
_cell_measurement_reflns_used    8103
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.208
_cell_measurement_theta_min      2.233
_cell_volume                     8209.6(7)
_computing_cell_refinement
'SAINT+ in APEX2 v. 2008.4 (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, 2017)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX DUO 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  0.0640
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            43738
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.286
_diffrn_reflns_theta_min         0.941
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.763
_exptl_absorpt_correction_T_max  0.5790
_exptl_absorpt_correction_T_min  0.3968
_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            colourless
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_description       prism
_exptl_crystal_F_000             4352
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.065
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         10107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0413P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7539
_reflns_number_total             10107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cy02353k2.cif
_cod_data_source_block           cmpnd_2
_cod_database_code               1550934
_shelxl_version_number           2014-3
_shelx_res_checksum              39690