Highly selective solvent free catalysis of CO2 and CS2 fixation under mild conditions using electronically varied zinc complexes
Barman, Souvik; Bag, Jayanta; Das, Dhiraj; Pal, Kuntal; New Journal of Chemistry 47 (2023) 20952–20965; doi:10.1039/D3NJ04231F

data_7062835
_publ_section_title
;
 Highly selective solvent free catalysis of CO2 and CS2 fixation under
 mild conditions using electronically varied zinc complexes
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20952
_journal_page_last               20965
_journal_paper_doi               10.1039/D3NJ04231F
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C18 H13 Br N5 O2 Zn, C16 H36 N'
_chemical_formula_sum            'C34 H49 Br N6 O2 Zn'
_chemical_formula_weight         719.07
_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_block_doi                 10.5517/ccdc.csd.cc2g32vj
_audit_creation_date             2023-10-09
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-10-10 deposited with the CCDC.	2023-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                91.334(3)
_cell_angle_beta                 97.550(4)
_cell_angle_gamma                107.982(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5795(9)
_cell_length_b                   11.9384(12)
_cell_length_c                   18.0751(17)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    144.99
_cell_measurement_theta_max      34.10
_cell_measurement_theta_min      2.61
_cell_volume                     1741.6(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      144.99
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.805
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25538
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.665
_diffrn_reflns_theta_min         2.613
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.891
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.6141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0970 before and 0.0487 after correction.
The Ratio of minimum to maximum transmission is 0.8223.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       needle
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         12050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.8729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9486
_reflns_number_total             12050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04231f2.cif
_cod_data_source_block           3OMe
_cod_depositor_comments
'Adding full bibliography for 7062834--7062837.cif.'
_cod_database_code               7062835
_shelx_shelxl_version_number     2016/6
_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 Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B),
 C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16), C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C30(H30A,H30B,
 H30C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              67742
_olex2_submission_special_instructions 'No special instructions were received'