Binding Enabled Catalytic Activation of SO2 by Copper Koneramine Complexes at Ambient Conditions
Chahal, Manoj; Raje, Sakthi; Kotana, Gopichand; Angamuthu, Raja; Green Chemistry  (2019) –; doi:10.1039/C9GC02647A

data_7234614
_publ_section_title
;
 Binding Enabled Catalytic Activation of SO2 by Copper Koneramine
 Complexes at Ambient Conditions
;
_journal_name_full               'Green Chemistry'
_journal_paper_doi               10.1039/C9GC02647A
_journal_year                    2019
_chemical_formula_moiety         'C23 H32 Cl Cu N9, 2(C F3 O3 S)'
_chemical_formula_sum            'C25 H32 Cl Cu F6 N9 O6 S2'
_chemical_formula_weight         831.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-06 deposited with the CCDC.    2019-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                100.763(2)
_cell_angle_beta                 99.350(2)
_cell_angle_gamma                108.877(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4954(8)
_cell_length_b                   11.7314(11)
_cell_length_c                   19.2810(18)
_cell_measurement_reflns_used    6279
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.61
_cell_volume                     1734.2(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_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  0.0452
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21482
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.338
_diffrn_reflns_theta_min         2.215
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0903 before and 0.0468 after correction. The Ratio of minimum to maximum transmission is 0.9104. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       block
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.586
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         8622
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0819
_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^)+(0.1390P)^2^+6.2118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2246
_refine_ls_wR_factor_ref         0.2612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6094
_reflns_number_total             8622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9gc02647a2.cif
_cod_data_source_block           5-[Cu(L-H)(H+)(OTf)Cl](OTf)
_cod_database_code               7234614
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.839
_shelx_estimated_absorpt_t_min   0.811
_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
 S0AA-C0AA
 1.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S0AA) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.05
Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.05
Uanis(C0AA) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.05
4.a Ternary CH refined with riding coordinates:
 C6(H6), C18(H18), C21(H21)
4.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C13(H13A,H13B), C7(H7A,H7B)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C2(H2), C1(H1), C12(H12), C10(H10), C3(H3), C4(H4), C11(H11), N8(H8),
 N7(H7), N9(H9A)
4.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              50238
_olex2_submission_special_instructions 'No special instructions were received'