Hydroboration of CO2 catalyzed by heteroscorpionate zwitterionic zinc and magnesium hydride complexes
He, Wenhao; Liu, Xinli; Cui, Dongmei; Dalton Transactions  (2022) –; doi:10.1039/D2DT00279E

data_7709675
_publ_section_title
;
 Hydroboration of CO2 catalyzed by heteroscorpionate zwitterionic zinc and
 magnesium hydride complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00279E
_journal_year                    2022
_chemical_formula_moiety         'C30 H31 N5 O2 P Zn, 2(C7 H8)'
_chemical_formula_sum            'C44 H47 N5 O2 P Zn'
_chemical_formula_weight         774.20
_chemical_name_systematic
'Heteroscorpionate Zwitterionic Zinc formate complex'
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_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     iterative
_audit_creation_date             2021-12-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-08 deposited with the CCDC.	2022-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                108.9870(10)
_cell_angle_beta                 97.2460(10)
_cell_angle_gamma                96.9120(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9364(6)
_cell_length_b                   12.6486(8)
_cell_length_c                   16.9877(11)
_cell_measurement_reflns_used    8207
_cell_measurement_temperature    173
_cell_measurement_theta_max      52.741
_cell_measurement_theta_min      5.145
_cell_volume                     1972.9(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'apex bruker'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0152
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11375
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.435
_diffrn_reflns_theta_min         1.728
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4047
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       cube
_exptl_crystal_F_000             814
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         7887
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0645P)^2^+1.2551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7343
_reflns_number_total             7887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00279e2.cif
_cod_data_source_block           g033m
_cod_database_code               7709675
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.816
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C37-C31
 1.51 with sigma of 0.02
 C31-C36 = C31-C32 = C35-C34
 1.39 with sigma of 0.02
 C36-C35 = C34-C33 = C33-C32
 1.38 with sigma of 0.02
 C51-C45
 1.51 with sigma of 0.02
 C45-C46 = C45-C50 = C47-C48
 1.39 with sigma of 0.02
 C46-C47 = C48-C49 = C49-C50
 1.38 with sigma of 0.02
 C31-C35
 2.42 with sigma of 0.04
 C36-C34
 2.39 with sigma of 0.04
 C31-C33
 2.41 with sigma of 0.04
 C35-C33 = C34-C32
 2.4 with sigma of 0.04
 C37-C36 = C37-C32
 2.52 with sigma of 0.04
 C47-C49 = C48-C50
 2.4 with sigma of 0.04
 C45-C49
 2.41 with sigma of 0.04
 C51-C46 = C51-C50
 2.52 with sigma of 0.04
 C45-C47
 2.42 with sigma of 0.04
 C46-C48
 2.39 with sigma of 0.04
 C31-C36 \\sim C36-C35 \\sim C35-C34 \\sim C34-C33 \\sim C33-C32 \\sim C32-C31
 with sigma of 0.02
 C31-C33 \\sim C31-C35 \\sim C32-C34 \\sim C36-C32 \\sim C35-C33 \\sim C36-C34
 with sigma of 0.04
 C37-C32 \\sim C37-C36
 with sigma of 0.04
 C45-C49 \\sim C45-C47 \\sim C50-C48 \\sim C46-C50 \\sim C47-C49 \\sim C46-C48
 with sigma of 0.04
 C51-C50 \\sim C51-C46
 with sigma of 0.04
 C45-C46 \\sim C46-C47 \\sim C47-C48 \\sim C48-C49 \\sim C49-C50 \\sim C50-C45
 with sigma of 0.02
3. Restrained planarity
 C37, C31, C36, C35, C34, C33, C32
 with sigma of 0.1
 C51, C45, C46, C47, C48, C49, C50
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C37 \\sim C31 \\sim C36 \\sim C35 \\sim C34 \\sim C33 \\sim C32: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C51 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C37, C31, C36, C35, C34, C33, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51, C45, C46, C47, C48, C49, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51, C45, C46, C50, C47, C49, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C31(0.5) C36(0.5) H36(0.5)
 C35(0.5) H35(0.5) C34(0.5) H34(0.5) C33(0.5) H33(0.5) C32(0.5) H32(0.5)
 C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C46(0.5) H46(0.5) C45(0.5) C50(0.5)
 H50(0.5) C49(0.5) H49(0.5) C48(0.5) H48(0.5) C47(0.5) H47(0.5)
7.a Ternary CH refined with riding coordinates:
 C11(H11)
7.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C19(H19), C23(H23), C8(H8), C3(H3), C25(H25), C20(H20), C28(H28),
 C21(H21), C14(H14), C29(H29), C17(H17), C22(H22), C27(H27), C15(H15), C30(H30),
  C26(H26), C16(H16), C40(H40), C41(H41), C42(H42), C43(H43), C39(H39),
 C36(H36), C35(H35), C34(H34), C33(H33), C32(H32), C46(H46), C50(H50), C49(H49),
  C48(H48), C47(H47)
7.c Fitted hexagon refined as free rotating group:
 C40(C41,C42,C43,C38,C39), C46(C45,C50,C49,C48,C47)
7.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C44(H44A,H44B,H44C), C37(H37A,H37B,H37C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              21586
_olex2_submission_special_instructions 'No special instructions were received'