Absolute structure determination of compounds with axial and planar chirality using the crystalline sponge method
Yoshioka, Shota; Inokuma, Yasuhide; Hoshino, Manabu; Sato, Takashi; Fujita, Makoto; Chem. Sci. 6 (2015) 3765–; doi:10.1039/C5SC01681A

data_1519637
_publ_section_title
;
 Absolute structure determination of compounds with axial and planar
 chirality using the crystalline sponge method
;
_journal_issue                   7
_journal_name_full               'Chem. Sci.'
_journal_page_first              3765
_journal_paper_doi               10.1039/C5SC01681A
_journal_volume                  6
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C87.64 H68.04 I12 N24 S0.62 Zn6'
_chemical_formula_weight         3392.41
_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'
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;
2015-03-11 deposited with the CCDC.
2015-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_measurement_reflns_used    13353
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.8890
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_molecular_graphics    'shelXle (Hubschle et al., 2011)'
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_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2332
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
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_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -42
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_diffrn_reflns_limit_k_min       -18
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_diffrn_reflns_theta_max         74.380
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_diffrn_source                   'sealed X-ray tube'
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            yellow
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             6351
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.874
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details
;
 Flack x determined using 7144 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.102(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         30123
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1555P)^2^+38.5837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2307
_refine_ls_wR_factor_ref         0.2612
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_reflns_friedel_fraction_max     0.945
_reflns_number_gt                20640
_reflns_number_total             30123
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_cod_depositor_comments
'Adding full bibliography for 1519634--1519639.cif.'
_cod_database_code               1519637
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