Kinetically Trapped Tetrahedral Cages via Alkyne Metathesis.
Lee, Semin; Yang, Anna; Moneypenny, 2nd, Timothy P; Moore, Jeffrey S.; Journal of the American Chemical Society 138 (2016) 2182–2185; doi:10.1021/jacs.6b00468

data_4130117
_publ_contact_author
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Kinetically Trapped Tetrahedral Cages via Alkyne Metathesis.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2182
_journal_page_last               2185
_journal_paper_doi               10.1021/jacs.6b00468
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C33 H33 I3, C H2 Cl2'
_chemical_formula_sum            'C34 H35 Cl2 I3'
_chemical_formula_weight         895.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
; 
? 
;
_cell_angle_alpha                75.3898(16)
_cell_angle_beta                 76.1879(16)
_cell_angle_gamma                70.6752(15)
_cell_formula_units_Z            2
_cell_length_a                   10.9584(5)
_cell_length_b                   11.0990(5)
_cell_length_c                   15.2278(7)
_cell_measurement_reflns_used    9338
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.24
_cell_volume                     1666.62(13)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/4, TWINABS V2012/1 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-4 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd50xsa
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            83949
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.353
_diffrn_reflns_theta_min         2.238
_exptl_absorpt_coefficient_mu    2.995
_exptl_absorpt_correction_T_max  0.62775
_exptl_absorpt_correction_T_min  0.47079
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_id                cd50xsa
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (4 -3 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.239
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00992(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         8297
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0177
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0136P)^2^+1.3112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0393
_refine_ls_wR_factor_ref         0.0402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7849
_reflns_number_total             8297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b00468_si_002.cif
_cod_data_source_block           cd50xsa
_cod_database_code               4130117
_shelx_estimated_absorpt_t_min   0.450
_shelx_estimated_absorpt_t_max   0.535
_shelxl_version_number           2014/6
_shelx_res_checksum              26886
_shelx_hkl_checksum              52169