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_1542555
_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_formula_moiety
'C36 H24 I6 N12 Zn3, C7 H4 Cl2, C14 H10 Cl4, 2.5(C3 H6)'
_chemical_formula_sum            'C69 H62.5 Cl6 I6 N12 Zn3'
_chemical_formula_weight         2230.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 104.141(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.7365(13)
_cell_length_b                   15.0610(5)
_cell_length_c                   30.9345(11)
_cell_measurement_reflns_used    63645
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.468
_cell_measurement_theta_min      2.99
_cell_volume                     16145.3(11)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'RIGAKU VARIMAX with RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            88524
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.989
_diffrn_source                   X-ray
_exptl_absorpt_coefficient_mu    3.424
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4967
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_description       block
_exptl_crystal_F_000             8564
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.663
_refine_diff_density_min         -1.415
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         17652
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1421P)^2^+63.1154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2382
_refine_ls_wR_factor_ref         0.2736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9695
_reflns_number_total             17652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00594b2.cif
_cod_data_source_block           f2plus
_cod_depositor_comments
'Adding full bibliography for 1542555--1542557.cif.'
_cod_original_cell_volume        16145.2(11)
_cod_original_formula_sum        'C69 H62.50 Cl6 I6 N12 Zn3'
_cod_database_code               1542555
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.506
_shelx_estimated_absorpt_t_max   0.748
_shelx_res_checksum              65252
_shelx_hkl_checksum              69973