Thermally stable zinc hydride catalyst for hydrosilylation of CO2 to silyl formate at atmospheric pressure
Baalbaki, Hassan A.; Shu, Julia; Nyamayaro, Kudzanai; Jung, Hyuk-Joon; Mehrkhodavandi, Parisa; Chemical Communications  (2022) –; doi:10.1039/D2CC01498J

data_7130051
_publ_section_title
;
 Thermally stable zinc hydride catalyst for hydrosilylation of CO2 to
 silyl formate at atmospheric pressure
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01498J
_journal_year                    2022
_chemical_formula_moiety         'C41 H51 N2 O3 P Zn'
_chemical_formula_sum            'C41 H51 N2 O3 P Zn'
_chemical_formula_weight         716.17
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-07 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                72.988(3)
_cell_angle_beta                 75.997(3)
_cell_angle_gamma                83.549(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8580(13)
_cell_length_b                   13.1069(17)
_cell_length_c                   15.788(2)
_cell_measurement_reflns_used    9142
_cell_measurement_temperature    90
_cell_measurement_theta_max      33.13
_cell_measurement_theta_min      2.27
_cell_volume                     1890.8(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            74995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.330
_diffrn_reflns_theta_min         1.626
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0507 before and 0.0439 after correction.
The Ratio of minimum to maximum transmission is 0.9158.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.232
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         14497
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0453P)^2^+1.0191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11950
_reflns_number_total             14497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01498j2.cif
_cod_data_source_block           mo_pm294_0m
_cod_database_code               7130051
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.917
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3A-C41 \\sim O3B-C41
 with sigma of 0.02
3. Others
 Sof(H41A)=Sof(O3B)=1-FVAR(1)
 Sof(H41)=Sof(O3A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), C16(H16), C17(H17)
4.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
  C41(H41), C41(H41A)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              79155
_olex2_submission_special_instructions 'No special instructions were received'