Cycloelatanene A and B: absolute configuration determination and structural revision by the crystalline sponge method
Lee, Shoukou; Hoshino, Manabu; Fujita, Makoto; Urban, Sylvia; Chem. Sci. 8 (2017) 1547–; doi:10.1039/C6SC04288K

data_1544386
_publ_section_title
;
 Cycloelatanene A and B: absolute configuration determination and
 structural revision by the crystalline sponge method
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              1547
_journal_paper_doi               10.1039/C6SC04288K
_journal_volume                  8
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum
'C118.68 H134.52 Br0.86 Cl0.86 I12 N24 O1.71 Zn6'
_chemical_formula_weight         3938.17
_chemical_name_systematic
'Cycloelatanene B with ZnI2-TPT crystalline sponge'
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-22 deposited with the CCDC.
2016-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.611(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.2593(5)
_cell_length_b                   14.8434(1)
_cell_length_c                   31.0697(4)
_cell_measurement_reflns_used    95889
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.7040
_cell_measurement_theta_min      2.4330
_cell_volume                     15928.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'shelXle (Hubschle et al., 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'DECTRIS Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            146997
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.221
_diffrn_reflns_theta_min         2.525
_diffrn_source                   'Rigaku MicroMax 007HF rotating anode'
_exptl_absorpt_coefficient_mu    3.491
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro 1.171.38.41 was used'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       block
_exptl_crystal_F_000             7555
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 11844 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.033(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2231
_refine_ls_number_reflns         32337
_refine_ls_number_restraints     1400
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0575P)^2^+30.2001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.879
_reflns_number_gt                27619
_reflns_number_total             32337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04288k2.cif
_cod_data_source_block           SL-08_c-2
_cod_depositor_comments
'Adding full bibliography for 1544385--1544386.cif.'
_cod_database_code               1544386
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.375
_shelx_estimated_absorpt_t_max   0.679
_shelx_res_checksum              9868
_shelx_hkl_checksum              27193