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_7231639
_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         'C39 H42 N7, 3(I)'
_chemical_formula_sum            'C39 H42 I3 N7'
_chemical_formula_weight         989.49
_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             2017-11-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-07-04 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0824(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.34926(19)
_cell_length_b                   16.7927(2)
_cell_length_c                   36.5631(6)
_cell_measurement_reflns_used    10599
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.0100
_cell_measurement_theta_min      3.6280
_cell_volume                     8196.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7b (Rigaku OD, 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    '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 0.964
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -38.00 -11.75   0.35   26.50    --  -22.33 -82.00  17.00   75
  2  \w    -11.00  23.30   0.35   26.50    --  -22.33  82.00 139.00   98
  3  \w    -34.00   9.05   0.35   26.50    --   24.83 -82.00  17.00  123
  4  \w    -14.00  12.25   0.35   26.50    --  -22.33 -99.00 120.00   75
  5  \w     37.00  63.25   0.35   26.50    --   24.83 178.00 -60.00   75
  6  \w     35.00 107.10   0.35   26.50    --   24.83 178.00  90.00  206
  7  \w     44.00 110.85   0.35   26.50    --   24.83-178.00 -30.00  191
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0482035000
_diffrn_orient_matrix_UB_12      -0.0159070000
_diffrn_orient_matrix_UB_13      0.0036381000
_diffrn_orient_matrix_UB_21      -0.0180739000
_diffrn_orient_matrix_UB_22      -0.0168109000
_diffrn_orient_matrix_UB_23      0.0165195000
_diffrn_orient_matrix_UB_31      -0.0131227000
_diffrn_orient_matrix_UB_32      -0.0353472000
_diffrn_orient_matrix_UB_33      -0.0094924000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            37281
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.295
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.323
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7b (Rigaku Oxford Diffraction, 2015)
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_density_diffrn    1.604
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.112
_refine_diff_density_max         2.704
_refine_diff_density_min         -3.287
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         16019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.309
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1551P)^2^+19.6076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2348
_refine_ls_wR_factor_ref         0.2618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10910
_reflns_number_total             16019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01372a2.cif
_cod_data_source_block           nyy2017111402
_cod_depositor_comments
'Adding full bibliography for 7231632--7231641.cif.'
_cod_original_cell_volume        8196.4(2)
_cod_database_code               7231639
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C39H43N7O0.5I3
_reflns_odcompleteness_completeness 95.12
_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. Others
 Fixed Sof: I3(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B), C26(H26A,H26B),
 C27(H27A,H27B), C34(H34A,H34B), C36(H36A,H36B), C38(H38A,H38B), C8'(H8'A,H8'B),
  C9'(H9'A,H9'B), C17'(H17C,H17D), C18'(H18C,H18D), C26'(H26C,H26D), C27'(H27C,
 H27D), C34'(H34C,H34D), C36'(H36C,H36D), C38'(H38C,H38D)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C1'(H1'),
  C2'(H2'), C3'(H3'), C4'(H4'), C7'(H7'), C10'(H10'), C11'(H11'), C12'(H12'),
 C13'(H13'), C16'(H16'), C19'(H19'), C20'(H20'), C21'(H21'), C22'(H22'),
 C25'(H25')
3.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C35'(H35D,H35E,
 H35F), C37'(H37D,H37E,H37F), C39'(H39D,H39E,H39F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.089
_oxdiff_exptl_absorpt_empirical_full_min 0.919