Preparation and Characterization of a Halogen-Bonded Shape-Persistent Chiral Alleno-acetylenic Inclusion Complex.
Castro-Fernández, Silvia; Lahoz, Inmaculada R.; Llamas-Saiz, Antonio L; Alonso-Gómez, José Lorenzo; Cid, María-Magdalena; Navarro-Vázquez, Armando; Organic letters 16 (2014) 1136–1139; doi:10.1021/ol403778f

data_1513445
_publ_section_title
;
 Preparation and Characterization of a Halogen-Bonded Shape-Persistent
 Chiral Alleno-acetylenic Inclusion Complex.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              1136
_journal_page_last               1139
_journal_paper_doi               10.1021/ol403778f
_journal_volume                  16
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C70 H78 N2'
_chemical_formula_sum            'C70 H78 N2'
_chemical_formula_weight         947.34
_chemical_name_common            2011mg01mcf01
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-11-23T11:37:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.185(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.2464(15)
_cell_length_b                   6.8630(5)
_cell_length_c                   31.448(2)
_cell_measurement_reflns_used    4444
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.65
_cell_measurement_theta_min      1.49
_cell_measurement_wavelength     1.54178
_cell_volume                     6777.0(7)
_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      100(2)
_diffrn_detector_area_resol_mean 14
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '135mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD2000
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0095661
_diffrn_orient_matrix_UB_12      0.1330424
_diffrn_orient_matrix_UB_13      0.0054474
_diffrn_orient_matrix_UB_21      -0.02154
_diffrn_orient_matrix_UB_22      0
_diffrn_orient_matrix_UB_23      -0.0309054
_diffrn_orient_matrix_UB_31      -0.0214185
_diffrn_orient_matrix_UB_32      -0.0594204
_diffrn_orient_matrix_UB_33      0.0121968
_diffrn_radiation_monochromator  'multilayer confocal mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.083
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            51231
_diffrn_reflns_theta_full        54.65
_diffrn_reflns_theta_max         54.65
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.395
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.80085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;          
  Scalepak (Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         0.173
_refine_diff_density_min         -0.16
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.93
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         4573
_refine_ls_number_restraints     564
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0915P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1582
_reflns_number_gt                2563
_reflns_number_total             4573
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ol403778f_si_002.cif
_cod_data_source_block           PPPP-1
_cod_original_sg_symbol_H-M      C2
_cod_database_code               1513445