Bifunctional zinc and magnesium Schiff-base complexes containing quaternary ammonium side-arms for epoxide/CO<sub>2</sub> coupling reactions.
Virachotikul, Arnut; Laiwattanapaisarn, Nattiya; Chainok, Kittipong; Phomphrai, Khamphee; Dalton transactions (Cambridge, England : 2003) 50 (2021) 12399–12403; doi:10.1039/d1dt02121d

data_7707850
_publ_section_title
;
 Bifunctional zinc and magnesium Schiff-base complexes containing
 quaternary ammonium side-arms for epoxide/CO<sub>2</sub> coupling
 reactions.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12399
_journal_page_last               12403
_journal_paper_doi               10.1039/d1dt02121d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C23 H40 Cl1.851 I0.149 N2 O Zn, C H2 Cl2'
_chemical_formula_sum            'C24 H42 Cl3.85 I0.15 N2 O Zn'
_chemical_formula_weight         595.25
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_creation_date             2021-03-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-20 deposited with the CCDC.	2021-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.600(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4677(7)
_cell_length_b                   8.8859(4)
_cell_length_c                   24.3901(13)
_cell_measurement_reflns_used    9703
_cell_measurement_temperature    135.62
_cell_measurement_theta_max      26.361
_cell_measurement_theta_min      2.439
_cell_volume                     2915.8(3)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      135.62
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            79140
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.468
_diffrn_reflns_theta_min         2.306
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0933 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.8626.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             1245
_exptl_crystal_recrystallization_method
'recrystallization using dichlroromethane as solvent'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5996
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+2.6611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5211
_reflns_number_total             5996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02121d2.cif
_cod_data_source_block           kpav_catjk2al
_cod_depositor_comments          'Adding full bibliography for 7707850.cif.'
_cod_database_code               7707850
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.753
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Cl2A, I1}
{Cl1A, I2}
3. Restrained distances
 Zn1A-Cl1A \\sim Zn1A-Cl2A
 with sigma of 0.02
 Cl1-Cl2 \\sim Cl3-Cl4
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C24A: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Cl2 \\sim Cl4: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
Uanis(Cl2A) = Uanis(I1)
Uanis(Cl1A) = Uanis(I2)
5. Rigid body (RIGU) restrains
 N1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, Zn1A, N1, Cl2A, Cl1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, Cl2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl3, C24A, Cl4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(I1)=1-FVAR(1)
 Sof(Cl2A)=FVAR(1)
 Sof(I2)=1-FVAR(2)
 Sof(Cl1A)=FVAR(2)
 Sof(H24C)=Sof(H24D)=Sof(Cl3)=Sof(Cl4)=1-FVAR(3)
 Sof(Cl1)=Sof(Cl2)=Sof(H24A)=Sof(H24B)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C18(H18A,H18B), C20(H20A,H20B), C22(H22A,H22B),
 C24A(H24A,H24B), C24A(H24C,H24D)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7)
7.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C21(H21A,
 H21B,H21C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              93224
_shelx_hkl_checksum              34425
_olex2_submission_special_instructions 'No special instructions were received'