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_4127977
_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_sum            'Cl6 H36 O49 Zr4'
_chemical_formula_weight         1397.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.8320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4563(3)
_cell_length_b                   21.6794(6)
_cell_length_c                   17.1366(4)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.60
_cell_measurement_theta_min      3.29
_cell_volume                     3884.22(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31640
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.644
_diffrn_reflns_theta_max         66.644
_diffrn_reflns_theta_min         3.287
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    13.754
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.390
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.130
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         6864
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+11.0219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5999
_reflns_number_total             6864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08627_si_004.cif
_cod_data_source_block           cu_dk160_0m
_cod_database_code               4127977
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.446
_shelx_estimated_absorpt_t_max   0.683
_shelx_res_checksum              2592
_shelx_hkl_checksum              60280