N⋯I halogen bonding supported stabilization of a discrete pseudo-linear [I12]2−polyiodide
Peuronen, Anssi; Rinta, Heikki; Lahtinen, Manu; CrystEngComm 17 (2015) 1736–; doi:10.1039/C4CE01866D

data_7218348
_publ_section_title
;
 N&#x22EF;I halogen bonding supported stabilization of a discrete
 pseudo-linear [I12]2&#x2212;polyiodide
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1736
_journal_paper_doi               10.1039/C4CE01866D
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C18 H36 N4, 2(I5), 5(I2)'
_chemical_formula_sum            'C18 H36 I20 N4'
_chemical_formula_weight         2846.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                92.225(4)
_cell_angle_beta                 94.475(4)
_cell_angle_gamma                92.593(4)
_cell_formula_units_Z            1
_cell_length_a                   9.2353(4)
_cell_length_b                   9.5741(4)
_cell_length_c                   15.2398(7)
_cell_measurement_reflns_used    5229
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      28.8410
_cell_measurement_theta_min      3.1440
_cell_volume                     1340.80(10)
_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, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -61.00   32.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -        9.5778  -57.0000 -180.0000 93

  2 omega  -20.00   50.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -        9.5778  -99.0000   90.0000 70

  3 omega  -18.00   77.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -        9.5778   57.0000  -30.0000 95
;
_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      0.0063286000
_diffrn_orient_matrix_UB_12      0.0267379000
_diffrn_orient_matrix_UB_13      0.0442653000
_diffrn_orient_matrix_UB_21      -0.0690381000
_diffrn_orient_matrix_UB_22      -0.0317071000
_diffrn_orient_matrix_UB_23      0.0064888000
_diffrn_orient_matrix_UB_31      0.0338006000
_diffrn_orient_matrix_UB_32      -0.0615600000
_diffrn_orient_matrix_UB_33      0.0134876000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8950
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.148
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.553
_exptl_absorpt_correction_T_max  0.206
_exptl_absorpt_correction_T_min  0.059
_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            'metallic blackish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.525
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.1792
_exptl_crystal_size_min          0.1153
_refine_diff_density_max         1.142
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.252
_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     190
_refine_ls_number_reflns         5226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0162P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4473
_reflns_number_total             5226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce01866d2.cif
_cod_data_source_block           1-2I2-I16_2-
_cod_depositor_comments
'Adding full bibliography for 7218347--7218353.cif.'
_cod_database_code               7218348
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C18 H36 N4 I20'
_reflns_odcompleteness_completeness 98.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
;
_olex2_submission_special_instructions 'No special instructions were received'