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_7123696
_publ_section_title
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 A diquat-contained macrocyclic anion acceptor in pure water
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03750K
_journal_year                    2019
_chemical_formula_moiety         '4(F6 P), C44 H40 N8 O4, C2 H3 N'
_chemical_formula_sum            'C46 H43 F24 N9 O4 P4'
_chemical_formula_weight         1365.77
_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     dual
_audit_creation_date             2018-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2019-04-09 deposited with the CCDC.    2019-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                115.767(7)
_cell_angle_beta                 91.170(8)
_cell_angle_gamma                91.512(7)
_cell_formula_units_Z            2
_cell_length_a                   11.6025(11)
_cell_length_b                   16.878(2)
_cell_length_c                   17.2459(18)
_cell_measurement_reflns_used    3366
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      46.849
_cell_measurement_theta_min      4.247
_cell_volume                     3038.4(6)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.01
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1747
_diffrn_reflns_av_unetI/netI     0.2280
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33945
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.306
_diffrn_reflns_theta_min         4.245
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.459
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.3328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1467 before and 0.0929 after correction. The Ratio of minimum to maximum transmission is 0.4433. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       prism
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.208
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.0048(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         11498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.2428
_refine_ls_R_factor_gt           0.1467
_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^)+(0.0500P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3276
_refine_ls_wR_factor_ref         0.3903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4672
_reflns_number_total             11498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03750k2.cif
_cod_data_source_block           wmj18156
_cod_original_cell_volume        3038.5(6)
_cod_database_code               7123696
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.844
_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:
 C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C22(H22A,H22B), C34(H34A,H34B),
 C35(H35A,H35B), C37(H37A,H37B), C44(H44A,H44B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C6(H6), C9(H9), C11(H11), C12(H12), C14(H14),
 C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C25(H25), C26(H26), C27(H27),
  C30(H30), C31(H31), C33(H33), C36(H36), C39(H39), C40(H40), C42(H42), C43(H43)
2.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C)
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_shelx_res_checksum              92703
_shelx_fab_checksum              60396
_olex2_submission_special_instructions 'No special instructions were received'