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_1544385
_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 rm
_chemical_formula_sum
'C114.7 H129.68 Br0.47 Cl3.14 I12 N24 O0.93 Zn6'
_chemical_formula_weight         3922.89
_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
;
2016-10-24 deposited with the CCDC.
2016-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.739(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.1845(11)
_cell_length_b                   14.8561(2)
_cell_length_c                   31.0855(8)
_cell_measurement_reflns_used    19686
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.5010
_cell_measurement_theta_min      4.1760
_cell_volume                     15908.7(7)
_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    'shelxe (Hubschle et al., 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3040
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            81265
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.241
_diffrn_reflns_theta_min         3.656
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.267
_exptl_absorpt_correction_T_max  0.417
_exptl_absorpt_correction_T_min  0.078
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            colorless
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       block
_exptl_crystal_F_000             7516
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 8195 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.264(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2186
_refine_ls_number_reflns         32528
_refine_ls_number_restraints     1390
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0542
_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^)+(0.1042P)^2^+8.9141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.1894
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                22204
_reflns_number_total             32528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04288k2.cif
_cod_data_source_block           exp_231_c
_cod_depositor_comments
'Adding full bibliography for 1544385--1544386.cif.'
_cod_original_formula_sum
'C114.70 H129.68 Br0.47 Cl3.14 I12 N24 O0.93 Zn6'
_cod_database_code               1544385
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              48734
_shelx_hkl_checksum              49144