Peroxide-Promoted Disassembly Reassembly of Zr-Polyoxocations.
Sommers, James A.; Hutchison, Danielle C.; Martin, Nicolas P.; Kozma, Karoly; Keszler, Douglas A.; Nyman, May; Journal of the American Chemical Society 141 (2019) 16894–16902; doi:10.1021/jacs.9b08627

data_4127978
_publ_section_title
;
 Peroxide-Promoted Disassembly Reassembly of Zr-Polyoxocations.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16894
_journal_page_last               16902
_journal_paper_doi               10.1021/jacs.9b08627
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '3(O24 Zr4), 24.03(Cl O4)'
_chemical_formula_sum            'Cl24.02 H96 O168.11 Zr12'
_chemical_formula_weight         4732.77
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7157(5)
_cell_length_b                   16.7157(5)
_cell_length_c                   27.2185(10)
_cell_measurement_reflns_used    2829
_cell_measurement_temperature    171
_cell_measurement_theta_max      66.320
_cell_measurement_theta_min      3.740
_cell_volume                     7605.2(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      171
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13981
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.630
_diffrn_reflns_theta_max         66.630
_diffrn_reflns_theta_min         3.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.694
_exptl_absorpt_correction_T_max  0.5842
_exptl_absorpt_correction_T_min  0.2984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1160 before and 0.0563 after correction. The Ratio of minimum to maximum transmission is 0.5108. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_description       block
_exptl_crystal_F_000             4659
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.246
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0729
_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^)+(0.1569P)^2^+29.8710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2106
_refine_ls_wR_factor_ref         0.2322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2489
_reflns_number_total             3457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08627_si_003.cif
_cod_data_source_block           cu_dk173_0m_a
_cod_original_cell_volume        7605.2(5)
_cod_database_code               4127978
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Others
 Fixed Sof: Cl1(0.425) Cl3(0.87) O2(0.425) O10(0.87) O3(0.85) O12(0.87)
 O9(0.87) O11(0.87) O1(0.425) O8(0.5) O15(0.33333) O14(0.33333) O7(0.5)
 Cl5(0.33333) O13(0.5) O19(0.5) O16(0.33333) O17(0.16667) O18(0.16667)
;
_shelx_res_checksum              13144
_shelx_hkl_checksum              71205
_shelx_fab_checksum              63693
_olex2_submission_special_instructions 'No special instructions were received'