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_7231632
_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         'C30 H33 N6, C30 H32 N6, 2(Cu2 I5), 2(O)'
_chemical_formula_sum            'C60 H69 Cu4 I10 N12 O2'
_chemical_formula_weight         2513.43
_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   mixed
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1q3g1b
_audit_creation_date             2017-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-26 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.628(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6659(3)
_cell_length_b                   43.0938(10)
_cell_length_c                   22.4966(6)
_cell_measurement_reflns_used    15189
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.5990
_cell_measurement_theta_min      3.7417
_cell_volume                     7754.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41k (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    'SIR2004 (Burla et al., 2007)'
_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 0.999
_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    -46.00   6.00   0.80    6.00    --  -33.50  37.00-120.00   65
  2  \w    -68.00 -34.40   0.80    6.00    --  -33.50 178.00 120.00   42
  3  \w    -50.00 -22.80   0.80    6.00    --  -33.50 -57.00 -60.00   34
  4  \w    -94.00 -62.00   0.80    6.00    --  -33.50 -57.00 -60.00   40
  5  \w   -107.00 -32.60   0.80    6.00    --  -33.50 178.00  60.00   93
  6  \w    -33.00  29.40   0.80    6.00    --   36.47 -37.00  90.00   78
  7  \w     74.00 109.20   0.80    6.00    --   36.47 178.00 150.00   44
  8  \w     29.00  54.60   0.80    6.00    --   36.47 -57.00  90.00   32
  9  \w     69.00 104.20   0.80    6.00    --   36.47 178.00-180.00   44
 10  \w    -31.00  -5.40   0.80    6.00    --   36.47 -57.00  60.00   32
 11  \w     25.00  76.20   0.80    6.00    --   36.47  57.00  30.00   64
 12  \w    -32.00   8.00   0.80    6.00    --   36.47 -57.00  90.00   50
 13  \w     76.00 107.20   0.80    6.00    --   36.47  37.00 -90.00   39
 14  \w     -3.00  22.60   0.80    6.00    --   36.47 -99.00 -90.00   32
 15  \w     15.00  60.60   0.80    6.00    --   36.47  37.00 -90.00   57
 16  \w      9.00  37.00   0.80    6.00    --   36.47 -57.00  60.00   35
 17  \w     44.00  88.00   0.80   30.00    --  108.00 -30.00 150.00   55
 18  \w     47.00 109.40   0.80   30.00    --  108.00 -61.00-120.00   78
 19  \w     48.00  94.40   0.80   30.00    --  108.00 -94.00  90.00   58
 20  \w     38.00  84.40   0.80   30.00    --  108.00 -94.00  60.00   58
 21  \w     55.00  82.20   0.80   30.00    --  108.00 -30.00-180.00   34
 22  \w     44.00  90.40   0.80   30.00    --  108.00 -45.00 -60.00   58
 23  \w     88.00 175.20   0.80   30.00    --  108.00  45.00 -60.00  109
 24  \w     37.00  75.40   0.80   30.00    --  108.00 -30.00 120.00   48
 25  \w     38.00  84.40   0.80   30.00    --  108.00 -30.00  60.00   58
 26  \w     41.00 135.40   0.80   30.00    --  108.00 -77.00-180.00  118
;
_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      -0.0249738000
_diffrn_orient_matrix_UB_12      0.0104525000
_diffrn_orient_matrix_UB_13      -0.0685759000
_diffrn_orient_matrix_UB_21      0.0727545000
_diffrn_orient_matrix_UB_22      0.0321001000
_diffrn_orient_matrix_UB_23      0.0262559000
_diffrn_orient_matrix_UB_31      0.1766631000
_diffrn_orient_matrix_UB_32      -0.0117469000
_diffrn_orient_matrix_UB_33      0.0106677000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13509
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.100
_diffrn_reflns_theta_max         67.100
_diffrn_reflns_theta_min         3.742
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    32.858
_exptl_absorpt_correction_T_max  0.263
_exptl_absorpt_correction_T_min  0.033
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41k (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    2.153
_exptl_crystal_description       prism
_exptl_crystal_F_000             4700
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.066
_refine_diff_density_max         2.616
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         13509
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0795
_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^)+(0.1657P)^2^+19.6445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2294
_refine_ls_wR_factor_ref         0.2373
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12237
_reflns_number_total             13509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01372a2.cif
_cod_data_source_block           nyy2017101003a_tw
_cod_depositor_comments
'Adding full bibliography for 7231632--7231641.cif.'
_cod_database_code               7231632
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C60H65N12I10Cu4
_shelx_estimated_absorpt_t_max   0.220
_shelx_estimated_absorpt_t_min   0.059
_reflns_odcompleteness_completeness 97.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7391(14)
 0.2609(14)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1) = Uanis(O1A)
4. Others
 Sof(O1A)=1-FVAR(1)
 Sof(O1)=FVAR(1)
 Fixed Sof: O2(0.5) O3(0.5)
5.a Riding coordinates:
 C56(H56A,H56B)
5.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C46(H46A,H46B), C47(H47A,H47B), C55(H55A,H55B),
 C57(H57A,H57B)
5.c 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),
 C11(H11), C13(H13), C15(H15), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C43(H43), C45(H45), C48(H48)
5.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C)
;
_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 1.391
_oxdiff_exptl_absorpt_empirical_full_min 0.819
_oxdiff_exptl_absorpt_spherical_max 0.142
_oxdiff_exptl_absorpt_spherical_min 0.053