N-Alkyl ammonium resorcinarene polyiodides
Pan, Fangfang; Beyeh, Ngong Kodiah; Ras, Robin H. A.; Rissanen, Kari; CrystEngComm 18 (2016) 5724–; doi:10.1039/C6CE01229A

data_7225583
_publ_section_title
;
 N-Alkyl ammonium resorcinarene polyiodides
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              5724
_journal_paper_doi               10.1039/C6CE01229A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C56 H88 N4 O8, I3, 2(C H4 O), 3(Br)'
_chemical_formula_sum            'C58 H96 Br3 I3 N4 O10'
_chemical_formula_weight         1629.81
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-26 deposited with the CCDC.
2016-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.343(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0087(4)
_cell_length_b                   27.3833(5)
_cell_length_c                   16.3215(4)
_cell_measurement_reflns_used    7741
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      72.1950
_cell_measurement_theta_min      3.1220
_cell_volume                     6706.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega -115.00   -5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.0263  -19.0000  120.0000 110

  2 omega   76.00  170.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   61.0000 -135.3851 94

  3 omega   69.00  170.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818   15.0000 -180.0000 101

  4 omega   29.00   91.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818  -30.0000  -90.0000 62

  5 omega -116.00  -18.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.0263  -37.0000  -90.0000 98

  6 omega  -83.00   38.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.0263   19.0000  -60.0000 121

  7 omega   32.00   57.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0818 -125.0000 -150.0000 25

  8 omega   24.00  108.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -94.0000  -90.0000 84

  9 omega   32.00   58.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -30.0000   60.0000 26

 10 omega   81.00  125.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601   45.0000  -60.0000 44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0775095000
_diffrn_orient_matrix_UB_12      0.0144240000
_diffrn_orient_matrix_UB_13      -0.0585594000
_diffrn_orient_matrix_UB_21      0.0127978000
_diffrn_orient_matrix_UB_22      -0.0476236000
_diffrn_orient_matrix_UB_23      -0.0485182000
_diffrn_orient_matrix_UB_31      -0.0660499000
_diffrn_orient_matrix_UB_32      -0.0262230000
_diffrn_orient_matrix_UB_33      0.0560428000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29031
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.748
_diffrn_reflns_theta_max         66.748
_diffrn_reflns_theta_min         3.153
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.511
_exptl_absorpt_correction_T_max  0.704
_exptl_absorpt_correction_T_min  0.340
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       needle
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.1561
_exptl_crystal_size_mid          0.0342
_exptl_crystal_size_min          0.0331
_refine_diff_density_max         2.691
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.175
_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     722
_refine_ls_number_reflns         11813
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0692
_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^)+(0.1297P)^2^+2.8734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1935
_refine_ls_wR_factor_ref         0.2275
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8064
_reflns_number_total             11813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01229a2.cif
_cod_data_source_block           2_Br3_I3
_cod_depositor_comments
'Adding full bibliography for 7225581--7225584.cif.'
_cod_database_code               7225583
_chemical_oxdiff_formula         'C60 H50 O8 N4 Br4 I3'
_reflns_odcompleteness_completeness 99.17
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C58-O10
 1.4 with sigma of 0.02
 H4-O5_$1
 2.3 with sigma of 0.02
 H53-H1
 2.15 with sigma of 0.02
 H4-H21A
 2.15 with sigma of 0.01
 H58B_$2-H28C
 2.15 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Riding coordinates:
 O9(H9)
4.b Ternary CH refined with riding coordinates:
 C11(H11), C25(H25), C39(H39), C53(H53)
4.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C13(H13A,H13B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B),
  C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C40(H40A,H40B), C41(H41A,
 H41B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C54(H54A,H54B),
 C55(H55A,H55B), N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B)
4.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C20(H20), C34(H34), C48(H48)
4.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C28(H28A,H28B,
 H28C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C52(H52A,H52B,H52C), C56(H56A,
 H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C)
4.f Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3), O4(H4), O5(H5), O6(H6A), O7(H7), O8(H8), O10(H10)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'