Cyclopropenium Cations Break the Rules of Attraction to Form Closely Bound Dimers.
Wallace, Andrew J.; Jayasinghe, Chaminda D.; Polson, Matthew I. J.; Curnow, Owen J.; Crittenden, Deborah L.; Journal of the American Chemical Society 137 (2015) 15528–15532; doi:10.1021/jacs.5b10388

data_4129765
_publ_section_title
;
 Cyclopropenium Cations Break the Rules of Attraction to Form Closely
 Bound Dimers.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15528
_journal_page_last               15532
_journal_paper_doi               10.1021/jacs.5b10388
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'I, C15 H30 N3'
_chemical_formula_sum            'C15 H30 I N3'
_chemical_formula_weight         379.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.431(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.4506(4)
_cell_length_b                   10.6276(3)
_cell_length_c                   19.3662(5)
_cell_measurement_reflns_used    8432
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.6080
_cell_measurement_theta_min      4.7200
_cell_volume                     3677.62(17)
_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      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_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      0.0267894500
_diffrn_orient_matrix_UB_12      -0.1350378500
_diffrn_orient_matrix_UB_13      -0.0086868000
_diffrn_orient_matrix_UB_21      -0.0196134500
_diffrn_orient_matrix_UB_22      0.0178347500
_diffrn_orient_matrix_UB_23      -0.0815588000
_diffrn_orient_matrix_UB_31      0.0795225000
_diffrn_orient_matrix_UB_32      0.0496425000
_diffrn_orient_matrix_UB_33      0.0049682000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14985
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.100
_diffrn_reflns_theta_min         4.716
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.615
_exptl_absorpt_correction_T_max  0.440
_exptl_absorpt_correction_T_min  0.224
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.1967
_exptl_crystal_size_mid          0.1095
_exptl_crystal_size_min          0.0949
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0234
_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^)+(0.0382P)^2^+1.5008P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3547
_reflns_number_total             3870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10388_si_003.cif
_cod_data_source_block           cham2ra
_cod_original_cell_volume        3677.61(16)
_cod_database_code               4129765
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C15H30N3I1
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C31(H31A,H31B), C11(H11A,H11B), C33(H33A,H33B), C21(H21A,
 H21B), C13(H13A,H13B)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C14(H14A,H14B,H14C), C24(H24A,H24B,H24C)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'