X-ray Structure Analysis of Ozonides by the Crystalline Sponge Method.
Yoshioka, Shota; Inokuma, Yasuhide; Duplan, Vincent; Dubey, Ritesh; Fujita, Makoto; Journal of the American Chemical Society 138 (2016) 10140–10142; doi:10.1021/jacs.6b05817

data_4130698
_publ_section_title
;
 X-ray Structure Analysis of Ozonides by the Crystalline Sponge Method.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10140
_journal_page_last               10142
_journal_paper_doi               10.1021/jacs.6b05817
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C65.34 H67.68 I6 N12 O4.82 Zn3'
_chemical_formula_weight         2055.73
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.176(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.5334(9)
_cell_length_b                   14.9227(3)
_cell_length_c                   30.6034(10)
_cell_measurement_reflns_used    16628
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      73.7820
_cell_measurement_theta_min      4.2040
_cell_volume                     15862.5(8)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Supernova, Dual, Cu at zero, AtlastS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            33769
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         3.432
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    19.797
_exptl_absorpt_correction_T_max  0.234
_exptl_absorpt_correction_T_min  0.032
_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    1.722
_exptl_crystal_description       Block
_exptl_crystal_F_000             7922
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.278
_refine_diff_density_min         -1.858
_refine_diff_density_rms         0.174
_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     1093
_refine_ls_number_reflns         13993
_refine_ls_number_restraints     872
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1276P)^2^+36.7176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.1845
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12589
_reflns_number_total             13993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05817_si_002.cif
_cod_data_source_block           exp_146
_cod_original_cell_volume        15862.5(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4130698
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.044
_shelx_estimated_absorpt_t_max   0.183
_shelx_res_checksum              41075
_shelx_hkl_checksum              17751