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_4501821
_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         'C36 H54 N9, 6(C6 F4 I2), 3(C2 H6 O), 3(Cl)'
_chemical_formula_sum            'C78 H72 Cl3 F24 I12 N9 O3'
_chemical_formula_weight         3268.6
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-03-08T13:12:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.9240(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0024(2)
_cell_length_b                   28.0603(4)
_cell_length_c                   23.8472(3)
_cell_measurement_reflns_used    22683
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      0.407
_cell_measurement_wavelength     0.71073
_cell_volume                     10033.3(2)
_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)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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      0.495344E-1
_diffrn_orient_matrix_UB_12      -0.10737E-2
_diffrn_orient_matrix_UB_13      -0.270044E-1
_diffrn_orient_matrix_UB_21      -0.158337E-1
_diffrn_orient_matrix_UB_22      0.328664E-1
_diffrn_orient_matrix_UB_23      -0.131299E-1
_diffrn_orient_matrix_UB_31      0.417573E-1
_diffrn_orient_matrix_UB_32      0.137362E-1
_diffrn_orient_matrix_UB_33      0.29305E-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  0.0421
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            70361
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.63
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.877
_exptl_absorpt_correction_T_max  0.4313
_exptl_absorpt_correction_T_min  0.3326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6120
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.325
_refine_diff_density_min         -3.291
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1168
_refine_ls_number_reflns         22959
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+122.4400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.163
_reflns_number_gt                16885
_reflns_number_total             22959
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg100516t_si_001.cif
_cod_data_source_block           1-HCl-F4DIB
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4501821