Structure determination of microbial metabolites by the crystalline sponge method
Inokuma, Yasuhide; Ukegawa, Tomoya; Hoshino, Manabu; Fujita, Makoto; Chem. Sci. 7 (2016) 3910–; doi:10.1039/C6SC00594B

data_1542557
_publ_section_title
;
 Structure determination of microbial metabolites by the crystalline
 sponge method
;
_journal_issue                   6
_journal_name_full               'Chem. Sci.'
_journal_page_first              3910
_journal_paper_doi               10.1039/C6SC00594B
_journal_volume                  7
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety
;
(C72 H48 I12 N24 Zn6), 2.805(C19 H26 O3), 1.5(C6 H12) 
;
_chemical_formula_sum            'C134.29 H138.92 I12 N24 O8.41 Zn6'
_chemical_formula_weight         4147.41
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-02-04 deposited with the CCDC.
2016-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.601(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.7707(6)
_cell_length_b                   14.8406(3)
_cell_length_c                   31.2152(5)
_cell_measurement_reflns_used    35702
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      73.3970
_cell_measurement_theta_min      2.9030
_cell_volume                     15719.6(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            106306
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.717
_diffrn_reflns_theta_min         2.604
_exptl_absorpt_coefficient_mu    19.976
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             8000
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.899
_refine_diff_density_min         -1.234
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details
;
 Flack x determined using 8301 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1842
_refine_ls_number_reflns         29574
_refine_ls_number_restraints     904
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0788
_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^)+(0.1699P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2091
_refine_ls_wR_factor_ref         0.2259
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.876
_reflns_Friedel_fraction_max     0.824
_reflns_number_gt                23414
_reflns_number_total             29574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00594b2.cif
_cod_data_source_block           SX312a_b
_cod_depositor_comments
'Adding full bibliography for 1542555--1542557.cif.'
_cod_database_code               1542557
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.071
_shelx_estimated_absorpt_t_max   0.335
_shelx_res_checksum              47856
_shelx_hkl_checksum              42294