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_4515595
_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         'C21 H35 N3 Zn, 0.25(C6 H14)'
_chemical_formula_sum            'C22.5 H38.5 N3 Zn'
_chemical_formula_weight         416.47
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2017-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.482(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8856(3)
_cell_length_b                   21.7310(4)
_cell_length_c                   16.0804(2)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      60.58
_cell_measurement_theta_min      4.53
_cell_volume                     4770.90(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.9903
_diffrn_measured_fraction_theta_max 0.9903
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35462
_diffrn_reflns_theta_full        60.5849
_diffrn_reflns_theta_max         60.58
_diffrn_reflns_theta_min         2.82
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.915
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.6000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1112 before and 0.0492 after correction.
The Ratio of minimum to maximum transmission is 0.7980.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.1596
_exptl_crystal_description       block
_exptl_crystal_F_000             1776.4891
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.8231
_refine_diff_density_min         -0.4839
_refine_diff_density_rms         0.0566
_refine_ls_d_res_high            0.7700
_refine_ls_d_res_low             13.6529
_refine_ls_goodness_of_fit_ref   1.0408
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    110
_refine_ls_number_parameters     502
_refine_ls_number_reflns         10837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0408
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+2.0177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -19
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                9249
_reflns_number_total             10837
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            cs8b01033_si_002.cif
_cod_data_source_block           L1ZnH
_cod_database_code               4515595
_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:
 C16(H16), C19(H19), C37(H37), C40(H40)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C7(H7a,H7b), C27(H27a,H27b), C28(H28a,H28b), C44(H44a,H44b),
 C45(H45a,H45b)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C12(H12), C13(H13), C14(H14), C33(H33), C34(H34), C35(H35), C24(H24)
2.d Idealised Me refined as rotating group:
 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),
 C22(H22a,H22b,H22c), C26(H26a,H26b,H26c), C29(H29a,H29b,H29c), C30(H30a,H30b,
 H30c), C38(H38a,H38b,H38c), C39(H39a,H39b,H39c), C41(H41a,H41b,H41c), C42(H42a,
 H42b,H42c), C43(H43a,H43b,H43c)
;
_olex2_submission_special_instructions 'No special instructions were received'