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_4130696
_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            'C52.6 H59.36 I6.02 N12 O2.55 Zn3'
_chemical_formula_weight         1860.31
_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                 99.307(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.440(2)
_cell_length_b                   14.9178(8)
_cell_length_c                   29.894(2)
_cell_measurement_reflns_used    5953
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      71.9610
_cell_measurement_theta_min      4.2660
_cell_volume                     15156.4(16)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            27681
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         3.636
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    20.681
_exptl_absorpt_correction_T_max  0.250
_exptl_absorpt_correction_T_min  0.063
_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    1.630
_exptl_crystal_description       Block
_exptl_crystal_F_000             7107
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.999
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.000063(8)
_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   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     881
_refine_ls_number_reflns         13377
_refine_ls_number_restraints     1282
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1350
_refine_ls_R_factor_gt           0.0969
_refine_ls_shift/su_max          1.829
_refine_ls_shift/su_mean         0.037
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1407P)^2^+121.7301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2784
_refine_ls_wR_factor_ref         0.3075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7726
_reflns_number_total             13377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05817_si_005.cif
_cod_data_source_block           exp_437_a
_cod_original_cell_volume        15156.7(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C52.60 H59.36 I6.02 N12 O2.55 Zn3'
_cod_database_code               4130696
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.037
_shelx_estimated_absorpt_t_max   0.190
_shelx_res_checksum              64755
_shelx_hkl_checksum              48881