The conformational behavior of multivalent tris(imidazolium)cyclophanes in the hybrids with metal (pseudo)halides or polyoxometalates
Wang, Fu-Rong; Li, Zi-Yan; Wei, Dong-Hui; Niu, Yun-Yin; Hou, Hong-Wei; Wu, Ben-Lai; CrystEngComm 20 (2018) 7184–; doi:10.1039/C8CE01372A

data_7231633
_publ_section_title
;
 The conformational behavior of multivalent tris(imidazolium)cyclophanes
 in the hybrids with metal (pseudo)halides or polyoxometalates
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              7184
_journal_paper_doi               10.1039/C8CE01372A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety
'Ag C4 N4 S4, C33 H39 N6, 0.5(C4 H6 N2), 2(H2 O)'
_chemical_formula_sum            'C39 H46 Ag N11 O2 S4'
_chemical_formula_weight         936.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-01 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7409(5)
_cell_length_b                   17.1057(3)
_cell_length_c                   11.6678(2)
_cell_measurement_reflns_used    3761
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.8310
_cell_measurement_theta_min      4.3400
_cell_volume                     4139.59(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -87.00  -61.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -19.0000    0.0000 52

  2 omega  -80.00   -6.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -77.0000  -60.0000 148

  3 omega  -31.00   -5.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -19.0000    0.0000 52

  4 omega  -25.00   43.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -37.0000  -60.0000 136

  5 omega   60.00   86.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000 -150.0000 52

  6 omega   42.00   73.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  -60.0000 62

  7 omega   60.00  104.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000  -90.0000 88

  8 omega   25.00   54.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000  -90.0000 58

  9 omega   37.00  103.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -30.0000 132

 10 omega   89.00  167.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  150.0000 156

 11 omega   42.00   85.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -180.0000 86

 12 omega   44.00   71.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 54

 13 omega   37.00   91.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 108

 14 omega   67.00  124.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000 -120.0000 114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0169638000
_diffrn_orient_matrix_UB_12      0.0009720000
_diffrn_orient_matrix_UB_13      -0.1284986000
_diffrn_orient_matrix_UB_21      -0.0714538000
_diffrn_orient_matrix_UB_22      -0.0142576000
_diffrn_orient_matrix_UB_23      -0.0298836000
_diffrn_orient_matrix_UB_31      -0.0116208000
_diffrn_orient_matrix_UB_32      0.0888681000
_diffrn_orient_matrix_UB_33      -0.0034806000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10590
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.349
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.196
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       plate
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.3233
_exptl_crystal_size_mid          0.1313
_exptl_crystal_size_min          0.0211
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         3902
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0682
_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^)+(0.0876P)^2^+10.7609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.1931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3347
_reflns_number_total             3902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01372a2.cif
_cod_data_source_block           nyy2018011503
_cod_depositor_comments
'Adding full bibliography for 7231632--7231641.cif.'
_cod_original_cell_volume        4139.61(14)
_cod_database_code               7231633
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C39H46O2N11S4Ag1
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: H8A(0.5) H8B(0.5) H11A(0.5) H11B(0.5) H11C(0.5) H16A(0.5)
 H16B(0.5) H19A(0.5) H19B(0.5) H19C(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
4.a Free rotating group:
 O1(H1A,H1B)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C16(H16A,H16B), C18(H18A,H18B)
4.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C27(H27A,H27B,H27C)
;
_olex2_submission_special_instructions 'No special instructions were received'