A diquat-contained macrocyclic anion acceptor in pure water
Lei, Ye; Shen, Libo; Liu, Ji-Ren; Jiao, Tianyu; Zhang, Yang; Zhang, Chi; tong, lu; Hong, Xin; Pan, Yuanjiang; Li, Hao; Chemical Communications  (2019) –; doi:10.1039/C9CC03750K

data_7123695
_publ_section_title
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 A diquat-contained macrocyclic anion acceptor in pure water
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03750K
_journal_year                    2019
_chemical_formula_moiety         '4(Cl), C44 H40 N8 O4'
_chemical_formula_sum            'C44 H40 Cl4 N8 O4'
_chemical_formula_weight         886.64
_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     direct
_audit_creation_date             2019-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-06-10 deposited with the CCDC.    2019-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                89.490(12)
_cell_angle_beta                 79.110(11)
_cell_angle_gamma                84.227(13)
_cell_formula_units_Z            2
_cell_length_a                   10.5445(18)
_cell_length_b                   14.095(2)
_cell_length_c                   17.622(3)
_cell_measurement_reflns_used    2275
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      50.81
_cell_measurement_theta_min      3.55
_cell_volume                     2558.7(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.02
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.2064
_diffrn_reflns_av_unetI/netI     0.2731
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28278
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.582
_diffrn_reflns_theta_min         4.619
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.608
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.3290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1501 before and 0.0875 after correction. The Ratio of minimum to maximum transmission is 0.4382. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.732
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       0.050(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9697
_refine_ls_number_restraints     456
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.2672
_refine_ls_R_factor_gt           0.1609
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3664
_refine_ls_wR_factor_ref         0.4500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3523
_reflns_number_total             9697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03750k2.cif
_cod_data_source_block           mj19075_0m
_cod_original_cell_volume        2558.8(7)
_cod_database_code               7123695
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.856
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C21(H30A,H30B), C38(H42A,H42B), C30(H43A,H43B), C1(H45A,H45B), C20(H51A,H51B),
  C37(H54A,H54B), C23(H59A,H59B), C8(H68A,H68B)
3.b Aromatic/amide H refined with riding coordinates:
 C17(H3), C41(H14), C11(H16), C33(H18), C31(H26), C34(H27), C40(H29), C19(H32),
  C16(H33), C13(H41), C35(H46), C9(H48), C43(H49), C22(H52), C12(H56), C25(H61),
  C27(H77), C29(H63), C26(H69), C6(H72), C7(H47), C3(H12), C4(H55), C44(H78)
3.c Fitted hexagon refined as free rotating group:
 C25(C27,C28,C29,C26,C24), C5(C6,C7,C2,C3,C4)
;
_shelx_res_checksum              85031
_shelx_fab_checksum              87689
_olex2_submission_special_instructions 'No special instructions were received'