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_4130697
_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            'C60.08 H52.04 I6 N12 O4.47 Zn3'
_chemical_formula_weight         1971.08
_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                 101.858(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.8492(12)
_cell_length_b                   14.8584(5)
_cell_length_c                   31.0351(10)
_cell_measurement_reflns_used    9550
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      71.8770
_cell_measurement_theta_min      4.1860
_cell_volume                     15727.1(9)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            32570
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.137
_diffrn_reflns_theta_min         4.178
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    19.937
_exptl_absorpt_correction_T_max  0.045
_exptl_absorpt_correction_T_min  0.045
_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    1.665
_exptl_crystal_description       Block
_exptl_crystal_F_000             7522
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.053
_refine_diff_density_min         -2.679
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1057
_refine_ls_number_reflns         15525
_refine_ls_number_restraints     1057
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0699
_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^)+(0.1144P)^2^+119.2248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2045
_refine_ls_wR_factor_ref         0.2142
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12960
_reflns_number_total             15525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05817_si_004.cif
_cod_data_source_block           datam
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4130697
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.066
_shelx_estimated_absorpt_t_max   0.218
_shelx_res_checksum              56586
_shelx_hkl_checksum              47351