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_4127976
_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         'H80 O110 Zr25'
_chemical_formula_sum            'H80 O110 Zr25'
_chemical_formula_weight         4121.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-13
_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            4
_cell_length_a                   31.6822(4)
_cell_length_b                   23.4638(2)
_cell_length_c                   27.1118(4)
_cell_measurement_reflns_used    73233
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.6560
_cell_measurement_theta_min      1.9060
_cell_volume                     20154.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -12.00  41.00   0.50   77.01    --   10.95  77.00  30.00  106
  2  \w    -12.00  41.00   0.50   77.01    --   10.95  77.00 120.00  106
  3  \w    -39.00  24.00   0.50   77.01    --  -12.35  86.00  93.74  126
  4  \w    -55.00 -24.00   0.50   77.01    --  -12.35 115.00 -67.97   62
  5  \w    -64.00   2.00   0.50   77.01    --   10.95 -19.00-180.00  132
  6  \w    -41.00 -12.00   0.50   77.01    --   10.95 -77.00 -60.00   58
  7  \w    -18.00  21.00   0.50   77.01    --  -12.35 -99.00  30.00   78
  8  \w    -84.00   3.00   0.50   77.01    --  -12.35 -57.00 150.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0045290000
_diffrn_orient_matrix_UB_12      -0.0042888000
_diffrn_orient_matrix_UB_13      0.0253463000
_diffrn_orient_matrix_UB_21      0.0218519000
_diffrn_orient_matrix_UB_22      -0.0013890000
_diffrn_orient_matrix_UB_23      -0.0055653000
_diffrn_orient_matrix_UB_31      0.0016542000
_diffrn_orient_matrix_UB_32      0.0298877000
_diffrn_orient_matrix_UB_33      0.0034003000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            141850
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.642
_diffrn_reflns_theta_min         1.891
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.332
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       plate
_exptl_crystal_F_000             7840
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.193
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         14706
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+114.2012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12744
_reflns_number_total             14706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08627_si_002.cif
_cod_data_source_block           run2
_cod_database_code               4127976
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Zr O H Cl'
_diffrn_oxdiff_ac4_digest_frames
;
01560591be25ff3ec4bd052390425d731e008420e50
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Zr6B-O23B = O23B-Zr7B
 2.17 with sigma of 0.02
 Zr8B-O25B
 2.17 with sigma of 0.02
3. Others
 Fixed Sof: Zr8A(0.2375) Zr7A(0.475) Zr6A(0.475) O25A(0.95) O24A(0.95)
 Zr7B(0.025) O23A(0.475) Zr6B(0.0125) O18A(0.5) O10B(0.5) O10A(0.5) O18B(0.5)
 O2B(0.25) O2A(0.25) Zr8B(0.025) O24B(0.05) O23B(0.05) O25B(0.025)
4.a Rotating group:
 O7W(H7WA,H7WB), O9W(H9WA,H9WB), O8W(H8WA,H8WB), O10W(H10A,H10B), O6W(H6WA,
 H6WB), O5W(H5WA,H5WB), O4W(H4WA,H4WB), O3W(H3WA,H3WB), O2W(H2WA,H2WB),
 O1W(H1WA,H1WB)
;
_shelx_res_checksum              98032
_shelx_hkl_checksum              57881
_shelx_fab_checksum              3995
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.697
_oxdiff_exptl_absorpt_empirical_full_min 0.708