Side Arm Twist on Zn-Catalyzed Hydrosilylative Reduction of CO2 to Formate and Methanol Equivalents with High Selectivity and Activity
Feng, Guoqin; Du, Chongyang; Xiang, Li; del Rosal, Iker; Li, Guangyu; Leng, Xuebing; Chen, Eugene Y.-X.; Maron, Laurent; Chen, Yaofeng; ACS Catalysis 8 (2018) 4710–; doi:10.1021/acscatal.8b01033

data_4515596
_publ_section_title
;
 Side Arm Twist on Zn-Catalyzed Hydrosilylative Reduction of CO2 to
 Formate and Methanol Equivalents with High Selectivity and Activity
;
_journal_issue                   5
_journal_name_full               'ACS Catalysis'
_journal_page_first              4710
_journal_paper_doi               10.1021/acscatal.8b01033
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         '0.5(C44 H70 N6 O4 Zn2)'
_chemical_formula_sum            'C22 H35 N3 O2 Zn'
_chemical_formula_weight         438.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 117.531(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.041(6)
_cell_length_b                   10.016(3)
_cell_length_c                   22.532(6)
_cell_measurement_reflns_used    3999
_cell_measurement_temperature    130
_cell_measurement_theta_max      23.840
_cell_measurement_theta_min      2.26
_cell_volume                     4611(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1091
_diffrn_reflns_av_unetI/netI     0.1104
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            36431
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.660
_diffrn_reflns_theta_min         1.808
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.086
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1114 before and 0.0710 after correction.
The Ratio of minimum to maximum transmission is 0.6054.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.323
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         10649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0536
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6096
_reflns_number_total             10649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b01033_si_002.cif
_cod_data_source_block           L1ZnO2CH
_cod_database_code               4515596
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.854
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C38(H38), C41(H41), C16(H16), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C6(H6A,H6B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C34(H34), C35(H35), C36(H36), C44(H44), C3(H3), C12(H12), C13(H13),
 C14(H14), C22(H22)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
  C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C)
;
_shelx_res_checksum              4392
_shelx_hkl_checksum              4258
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'