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_7231636
_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, 3(I), 3(H2 O)'
_chemical_formula_sum            'C30 H39 I3 N6 O3'
_chemical_formula_weight         912.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2017-10-25
_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                 111.852(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7246(3)
_cell_length_b                   18.8111(5)
_cell_length_c                   11.1783(4)
_cell_measurement_reflns_used    2696
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.4080
_cell_measurement_theta_min      3.8760
_cell_volume                     1702.76(11)
_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   35.00   73.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       17.9098  178.0000 -120.0000 76

  2 omega  -34.00   64.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       17.9098    0.0000  -30.0000 196

  3 omega  -47.00   24.00   0.5000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       17.9098  -37.0000  -60.0000 142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0470885000
_diffrn_orient_matrix_UB_12      0.0236262000
_diffrn_orient_matrix_UB_13      -0.0221112000
_diffrn_orient_matrix_UB_21      -0.0560818000
_diffrn_orient_matrix_UB_22      -0.0049800000
_diffrn_orient_matrix_UB_23      -0.0643314000
_diffrn_orient_matrix_UB_31      -0.0480443000
_diffrn_orient_matrix_UB_32      0.0289640000
_diffrn_orient_matrix_UB_33      0.0069722000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7242
_diffrn_reflns_point_group_measured_fraction_full 0.772
_diffrn_reflns_point_group_measured_fraction_max 0.761
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         3.347
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.792
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91915
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 1096 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5278
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0103P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.479
_reflns_Friedel_fraction_full    0.532
_reflns_Friedel_fraction_max     0.509
_reflns_number_gt                4280
_reflns_number_total             5278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01372a2.cif
_cod_data_source_block           nyy2017102304
_cod_depositor_comments
'Adding full bibliography for 7231632--7231641.cif.'
_cod_database_code               7231636
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C20H20N1O5I2Ag1
_shelx_estimated_absorpt_t_max   0.768
_shelx_estimated_absorpt_t_min   0.713
_reflns_odcompleteness_completeness 99.69
_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. Restrained distances
 H3B-O3
 0.9 with sigma of 0.02
 H3A-O3
 0.9 with sigma of 0.02
 O2-H2A
 0.9 with sigma of 0.02
 O2-H2B
 0.9 with sigma of 0.02
 O1-H1A
 0.9 with sigma of 0.02
 O1-H1B
 0.9 with sigma of 0.02
 H3A-H3B
 1.38 with sigma of 0.04
 H2A-H2B
 1.38 with sigma of 0.04
 H1B-H1A
 1.38 with sigma of 0.04
3.a Riding coordinates:
 O1(H1A,H1B), O3(H3A,H3B)
3.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C26(H26A,H26B), C28(H28A,
 H28B), C30(H30A,H30B)
3.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)
3.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C)
;
_olex2_submission_special_instructions 'No special instructions were received'