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_7231641
_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         '1.5(Br3 Cu), C39 H43 N7, C2 H3 N'
_chemical_formula_sum            'C41 H46 Br4.5 Cu1.5 N8'
_chemical_formula_weight         1105.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2a 2n'
_space_group_name_H-M_alt        'P n c a'
_symmetry_space_group_name_Hall  '-P 2a 2n'
_symmetry_space_group_name_H-M   'P n c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-12-08
_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
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9746(2)
_cell_length_b                   35.1240(5)
_cell_length_c                   16.4115(2)
_cell_measurement_reflns_used    7515
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.9700
_cell_measurement_theta_min      3.8170
_cell_volume                     9208.4(2)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -40.00   -1.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   57.0000  -30.0000 78

  2 omega  -77.00  -43.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000  -30.0000 68

  3 omega  -98.00  -47.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -57.0000   30.0000 102

  4 omega  -48.00  -23.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   37.0000  150.0000 50

  5 omega   57.00   89.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000   30.0000 64

  6 omega  -28.00    1.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -57.0000 -180.0000 58

  7 omega  -27.00   26.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -77.0000 -120.0000 106

  8 omega   79.00  110.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000 -180.0000 62

  9 omega    7.00   33.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -57.0000 -180.0000 52

 10 omega   31.00   57.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -77.0000 -120.0000 52

 11 omega  102.00  172.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -60.0000 140

 12 omega   42.00   90.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 96

 13 omega   38.00   92.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 108

 14 omega   42.00  104.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   90.0000 124

 15 omega  128.00  178.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000   90.0000 100

 16 omega   42.00   79.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000   90.0000 74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0950705000
_diffrn_orient_matrix_UB_12      0.0061799000
_diffrn_orient_matrix_UB_13      -0.0085482000
_diffrn_orient_matrix_UB_21      0.0105701000
_diffrn_orient_matrix_UB_22      -0.0417486000
_diffrn_orient_matrix_UB_23      -0.0269906000
_diffrn_orient_matrix_UB_31      -0.0123485000
_diffrn_orient_matrix_UB_32      0.0119927000
_diffrn_orient_matrix_UB_33      -0.0894571000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23157
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         4.062
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31115
_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_density_diffrn    1.595
_exptl_crystal_F_000             4392
_refine_diff_density_max         2.354
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         8215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.1331
_refine_ls_R_factor_gt           0.1272
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1068P)^2^+326.3012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3477
_refine_ls_wR_factor_ref         0.3506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7383
_reflns_number_total             8215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01372a2.cif
_cod_data_source_block           nyy2017120603
_cod_depositor_comments
'Adding full bibliography for 7231632--7231641.cif.'
_cod_original_formula_sum        'C41 H46 Br4.50 Cu1.50 N8'
_cod_database_code               7231641
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C20H56N2O3Br1Cu1
_reflns_odcompleteness_completeness 99.72
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Br4(0.5) Br5(0.5) Br6(0.5) Cu1(0.5)
3.a Ternary CH refined with riding coordinates:
 N1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C13(H13A,H13B), C21(H21A,H21B), C27(H27A,H27B), C11(H11A,H11B),
 C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1G(H1GA,H1GB), C1J(H1JA,H1JB)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C15(H15), C16(H16), C18(H18), C23(H23), C26(H26), C29(H29),
 C30(H30), C4(H4), C10(H10), C12(H12), C1A(H1AA), C1E(H1E), C1H(H1H)
3.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C1L(H1LA,H1LB,H1LC)
;
_olex2_submission_special_instructions 'No special instructions were received'