Halogen-Bonded Solvates of Tetrahaloethynyl Cavitands
Turunen, Lotta; Pan, Fangfang; Beyeh, Ngong Kodiah; Cetina, Mario; Trant, John; Ras, Robin H.A.; Rissanen, Kari; CrystEngComm  (2017) –; doi:10.1039/C7CE01118K

data_7228805
_publ_section_title
;
 Halogen-Bonded Solvates of Tetrahaloethynyl Cavitands
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01118K
_journal_year                    2017
_chemical_formula_moiety         'C64 H68 I4 O8, C2 H3 N'
_chemical_formula_sum            'C66 H71 I4 N O8'
_chemical_formula_weight         1513.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-06-14 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.6494(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2220(2)
_cell_length_b                   24.9361(3)
_cell_length_c                   18.1166(3)
_cell_measurement_reflns_used    8862
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      75.7550
_cell_measurement_theta_min      3.5320
_cell_volume                     6351.82(16)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9758
_diffrn_measurement_details
;
  1 omega  -42.00  -13.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   37.0000   30.0000 29

  2 omega  -49.00   30.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   37.0000  -60.0000 79

  3 omega  -50.00   -5.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  125.0000  -30.0000 45

  4 omega  -49.00   28.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   37.0000 -120.0000 77

  5 omega  -83.00  -56.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  125.0000  -30.0000 27

  6 omega   79.00  170.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -30.0000 91

  7 omega  120.00  170.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000 -150.0000 50

  8 omega  101.00  147.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000 -120.0000 46

  9 omega   61.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 30

 10 omega  106.00  132.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000 -120.0000 26

 11 omega   44.00  139.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000 -180.0000 95

 12 omega   37.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -180.0000 54

 13 omega   36.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   90.0000 62

 14 omega   27.00   61.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.6513 -125.0000  150.0000 34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0294556000
_diffrn_orient_matrix_UB_12      -0.0167759000
_diffrn_orient_matrix_UB_13      0.0751233000
_diffrn_orient_matrix_UB_21      -0.0532715000
_diffrn_orient_matrix_UB_22      -0.0488277000
_diffrn_orient_matrix_UB_23      -0.0380198000
_diffrn_orient_matrix_UB_31      0.0910559000
_diffrn_orient_matrix_UB_32      -0.0339581000
_diffrn_orient_matrix_UB_33      0.0176625000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25434
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.749
_diffrn_reflns_theta_max         66.749
_diffrn_reflns_theta_min         3.038
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.831
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.583
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.2143
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.1121
_refine_diff_density_max         1.967
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         11246
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0707P)^2^+20.7338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8938
_reflns_number_total             11246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01118k2.cif
_cod_data_source_block           2_mecn
_cod_original_cell_volume        6351.82(17)
_cod_database_code               7228805
_chemical_oxdiff_formula         'C80 H80 O8 Br4 N2'
_reflns_odcompleteness_completeness 99.98
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C10(H10), C20(H20), C30(H30), C40(H40)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C19(H19A,H19B), C29(H29A,H29B), C39(H39A,H39B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C47(H47A,H47B),
  C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C53(H53A,
 H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
 C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C26(H26), C36(H36)
3.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C52(H52A,H52B,H52C), C58(H58A,H58B,H58C), C64(H64A,H64B,
 H64C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              67719
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'