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_7225584
_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         '2.5(I2), 7(Br1), 2(C44 H64 N4 O12)'
_chemical_formula_sum            'C88 H128 Br7 I5 N8 O24'
_chemical_formula_weight         2875.85
_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_Hall           '-P 4a 2bc'
_space_group_name_H-M_alt        'P 4/n n c'
_symmetry_space_group_name_Hall  '-P 4a 2bc'
_symmetry_space_group_name_H-M   'P 4/n n c :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-05-20
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3868(2)
_cell_length_b                   12.3868(2)
_cell_length_c                   36.9094(11)
_cell_measurement_reflns_used    5069
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.3060
_cell_measurement_theta_min      3.7450
_cell_volume                     5663.1(2)
_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)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -117.00   -9.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  -77.0000 -150.0000 108

  2 omega   56.00   91.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -30.0000 35

  3 omega  100.00  170.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000    0.0000 70

  4 omega   57.00   91.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 34

  5 omega   51.00   98.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -90.0000 47

  6 omega   51.00   91.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 40

  7 omega -116.00  -17.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  -37.0000   30.0000 99

  8 omega  -49.00   33.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   37.0000 -180.0000 82

  9 omega   36.00   91.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -150.0000 55

 10 omega   36.00   61.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  120.0000 25
;
_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      -0.0170354000
_diffrn_orient_matrix_UB_12      0.0608261000
_diffrn_orient_matrix_UB_13      0.0359648000
_diffrn_orient_matrix_UB_21      -0.0088384000
_diffrn_orient_matrix_UB_22      0.1072889000
_diffrn_orient_matrix_UB_23      -0.0209206000
_diffrn_orient_matrix_UB_31      -0.1228286000
_diffrn_orient_matrix_UB_32      -0.0161345000
_diffrn_orient_matrix_UB_33      -0.0034898000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            16009
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.730
_diffrn_reflns_theta_max         66.730
_diffrn_reflns_theta_min         3.764
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.224
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.315
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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    1.687
_exptl_crystal_description       plate
_exptl_crystal_F_000             2828
_exptl_crystal_size_max          0.2824
_exptl_crystal_size_mid          0.1285
_exptl_crystal_size_min          0.0421
_refine_diff_density_max         2.044
_refine_diff_density_min         -4.022
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.1135
_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^)+(0.1800P)^2^+40.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3201
_refine_ls_wR_factor_ref         0.3311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2008
_reflns_number_total             2522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01229a2.cif
_cod_data_source_block           3_br3_5_i2_5
_cod_depositor_comments
'Adding full bibliography for 7225581--7225584.cif.'
_cod_original_cell_volume        5663.1(3)
_cod_database_code               7225584
_chemical_oxdiff_formula         'C8 H22 N2 Cl2'
_reflns_odcompleteness_completeness 99.87
_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. Others
 Fixed Sof: Br19(0.7) Br1(0.175)
3.a Riding coordinates:
 O172(H172)
3.b Ternary CH refined with riding coordinates:
 C153(H153)
3.c Secondary CH2 refined with riding coordinates:
 N58(H58A,H58B), C28(H28A,H28B), C74(H74A,H74B), C133(H13A,H13B)
3.d Aromatic/amide H refined with riding coordinates:
 C121(H121)
3.e Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C)
3.f Idealised tetrahedral OH refined as rotating group:
 O8(H8), O20(H20)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20