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_7123697
_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         'C7 H7 O3 S, 3(F6 P), C44 H40 N8 O4'
_chemical_formula_sum            'C51 H47 F18 N8 O7 P3 S'
_chemical_formula_weight         1350.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.4113(5)
_cell_length_b                   33.6611(11)
_cell_length_c                   20.8777(6)
_cell_measurement_reflns_used    5779
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      44.62
_cell_measurement_theta_min      2.93
_cell_volume                     12236.1(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      169.99
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_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  0.1249
_diffrn_reflns_av_unetI/netI     0.0894
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38555
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.008
_diffrn_reflns_theta_min         2.934
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.433
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1525 before and 0.0890 after correction. The Ratio of minimum to maximum transmission is 0.5729. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       prism
_exptl_crystal_F_000             5504
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.00028(10)
_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   1.318
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         6161
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.316
_refine_ls_R_factor_all          0.2111
_refine_ls_R_factor_gt           0.1307
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3618
_refine_ls_wR_factor_ref         0.4193
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2797
_reflns_number_total             6161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03750k2.cif
_cod_data_source_block           wmj18095_sq
_cod_database_code               7123697
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.870
_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. Rigid body (RIGU) restrains
 S1, O4, O3, C7, C5, C6, C1, C4, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) F9(0.75) F11(0.375) F10(0.375) F7(0.5)
 F6(0.5) C28(0.5) H28(0.5) C29(0.5) H29(0.5) C30(0.5) H30(0.5) C31(0.5) H31(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C26(H26A,H26B), C18(H18A,H18B), C11(H11A,H11B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C4(H4), C2(H2), C24(H24), C21(H21), C12(H12), C16(H16),
 C8(H8), C25(H25), C22(H22), C14(H14), C10(H10), C15(H15), C28(H28), C29(H29),
 C30(H30), C31(H31)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
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_shelx_res_checksum              69114
_shelx_fab_checksum              29331
_olex2_submission_special_instructions 'No special instructions were received'