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_1519639
_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            'C86.95 H64.82 I12 N24 O1.87 Zn6'
_chemical_formula_weight         3390.77
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-03-11 deposited with the CCDC.
2015-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.7920(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.627(4)
_cell_length_b                   15.0818(16)
_cell_length_c                   31.194(3)
_cell_measurement_reflns_used    9816
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      24.39
_cell_measurement_theta_min      2.24
_cell_volume                     15886(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            75901
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.760
_diffrn_reflns_theta_max         24.760
_diffrn_reflns_theta_min         1.206
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.260
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             6342
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_transmission_factor_max   0.7451
_exptl_transmission_factor_min   0.6147
_refine_diff_density_max         1.730
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.232
_refine_ls_abs_structure_details
; 
 Flack x determined using 7021 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.082(11)
_refine_ls_extinction_coef       0.00013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1441
_refine_ls_number_reflns         27131
_refine_ls_number_restraints     263
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0745
_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^)+(0.1606P)^2^+48.1577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2240
_refine_ls_wR_factor_ref         0.2548
_reflns_Friedel_coverage         0.916
_reflns_friedel_fraction_full    0.994
_reflns_friedel_fraction_max     0.994
_reflns_number_gt                18487
_reflns_number_total             27131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc01681a2.cif
_cod_data_source_block           c2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1519634--1519639.cif.
;
_cod_database_code               1519639
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.696
_shelx_estimated_absorpt_t_max   0.881
_shelx_res_checksum              24585
_shelx_hkl_checksum              51173