Modulation of N···I and+N−H···Cl−···I Halogen Bonding: Folding, Inclusion, and Self-Assembly of Tri- and Tetraamino Piperazine Cyclophanes
Raatikainen, Kari; Rissanen, Kari; Crystal Growth & Design 10 (2010) 3638–; doi:10.1021/cg100516t

data_4501822
_publ_section_title
;
 Modulation of N&#x00B7;&#x00B7;&#x00B7;I
 and+N&#x2212;H&#x00B7;&#x00B7;&#x00B7;Cl&#x2212;&#x00B7;&#x00B7;&#x00B7;I
 Halogen Bonding: Folding, Inclusion, and Self-Assembly of Tri- and
 Tetraamino Piperazine Cyclophanes
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3638
_journal_paper_doi               10.1021/cg100516t
_journal_volume                  10
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C48 H68 N12), C6 F4 I2, C H4 O, 2(C H CL3)'
_chemical_formula_sum            'C105 H142 Cl6 F4 I2 N24 O'
_chemical_formula_weight         2298.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-03-09T10:27:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.3560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7978(2)
_cell_length_b                   40.2212(6)
_cell_length_c                   20.7248(4)
_cell_measurement_reflns_used    25187
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      0.41
_cell_measurement_wavelength     0.71073
_cell_volume                     11468.3(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.293998E-1
_diffrn_orient_matrix_UB_12      -0.221019E-1
_diffrn_orient_matrix_UB_13      -0.88772E-2
_diffrn_orient_matrix_UB_21      -0.340891E-1
_diffrn_orient_matrix_UB_22      0
_diffrn_orient_matrix_UB_23      -0.443392E-1
_diffrn_orient_matrix_UB_31      0.570678E-1
_diffrn_orient_matrix_UB_32      0.113863E-1
_diffrn_orient_matrix_UB_33      -0.172316E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33562
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.01
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4768
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.325
_refine_diff_density_min         -1.532
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1329
_refine_ls_number_reflns         19256
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_gt           0.0905
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+104.4600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1936
_refine_ls_wR_factor_ref         0.2257
_reflns_number_gt                13934
_reflns_number_total             19256
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg100516t_si_001.cif
_cod_data_source_block           2-F4DIB
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4501822