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_7231634
_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         'C33 H39 N6, Hg I4, I'
_chemical_formula_sum            'C33 H39 Hg I5 N6'
_chemical_formula_weight         1354.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-09-13
_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                 125.510(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7081(3)
_cell_length_b                   16.2105(3)
_cell_length_c                   27.4270(8)
_cell_measurement_reflns_used    6918
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8490
_cell_measurement_theta_min      3.8790
_cell_volume                     3875.4(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -25.00   19.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -15.3317  -99.0000 -180.0000 88

  2 omega  -20.00   17.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -15.3317  -99.0000   60.0000 74

  3 omega  -13.00   30.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -77.0000    0.0000 86

  4 omega   -9.00   88.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661   19.0000  -30.0000 194

  5 omega   31.00   58.50   0.5000    8.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661   57.0000    0.0000 55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0439109000
_diffrn_orient_matrix_UB_12      -0.0333124000
_diffrn_orient_matrix_UB_13      0.0192396000
_diffrn_orient_matrix_UB_21      -0.0030992000
_diffrn_orient_matrix_UB_22      -0.0195987000
_diffrn_orient_matrix_UB_23      -0.0238103000
_diffrn_orient_matrix_UB_31      0.0684362000
_diffrn_orient_matrix_UB_32      0.0204813000
_diffrn_orient_matrix_UB_33      0.0085058000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            18683
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.441
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.986
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68501
_exptl_absorpt_correction_type   multi-scan
_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)
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    2.322
_exptl_crystal_description       prism
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0342P)^2^+3.9256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6561
_reflns_number_total             7907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01372a2.cif
_cod_data_source_block           nyy2017090603a
_cod_depositor_comments
'Adding full bibliography for 7231632--7231641.cif.'
_cod_original_cell_volume        3875.4(2)
_cod_database_code               7231634
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C38H41N2I2Hg1
_shelx_estimated_absorpt_t_max   0.380
_shelx_estimated_absorpt_t_min   0.298
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C10(H10A,H10B), C18(H18A,H18B), C20(H20A,H20B), C28(H28A,H28B), C30(H30A,
 H30B), C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C)
;
_olex2_submission_special_instructions 'No special instructions were received'