Zr6O8 core cluster with formula unit [Zr6O4(OH)4(OH2)8(CH3COO)4(SO4)4]·nH2O obtained under mild conditions
Garzón-Serrano, Andrea Y.; Lozano, Johan D.; Perez, Leon D.; Sierra, César A.; Macías, Mario A.; RSC Advances 14 (2024) 29910–29918; doi:10.1039/D4RA03940H

data_7249357
_publ_section_title
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 Zr6O8 core cluster with formula unit
 [Zr6O4(OH)4(OH2)8(CH3COO)4(SO4)4]&#x00B7;nH2O obtained under mild
 conditions
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_journal_issue                   41
_journal_name_full               'RSC Advances'
_journal_page_first              29910
_journal_page_last               29918
_journal_paper_doi               10.1039/D4RA03940H
_journal_volume                  14
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C8 H32 O40 S4 Zr6, 13[H2O]'
_chemical_formula_sum            'C8 H58 O53 S4 Zr6'
_chemical_formula_weight         1678.125
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_Int_Tables_number      9
_audit_creation_date             2024-08-12
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.08.07 svn.r83e07e25 for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-08-14 deposited with the CCDC.	2024-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.436(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9608(13)
_cell_length_b                   27.9958(19)
_cell_length_c                   14.7493(11)
_cell_measurement_reflns_used    3708
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      75.3770
_cell_measurement_theta_min      4.6130
_cell_volume                     5161.9(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean 10.6144
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9979
_diffrn_measured_fraction_theta_max 0.9773
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0795
_diffrn_reflns_Laue_measured_fraction_full 0.9979
_diffrn_reflns_Laue_measured_fraction_max 0.9773
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13189
_diffrn_reflns_point_group_measured_fraction_full 0.6621
_diffrn_reflns_point_group_measured_fraction_max 0.6453
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.09
_diffrn_reflns_theta_min         3.87
_exptl_absorpt_coefficient_mu    12.285
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             3350.454
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_platon_squeeze_details          )
_refine_diff_density_max         1.0548
_refine_diff_density_min         -0.9730
_refine_diff_density_rms         0.1436
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_d_res_high            0.7942
_refine_ls_d_res_low             11.4147
_refine_ls_goodness_of_fit_ref   1.0233
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    47
_refine_ls_number_parameters     538
_refine_ls_number_reflns         6972
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.0154
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          -0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0838P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1437
_reflns_Friedel_coverage         0.312
_reflns_limit_h_max              17
_reflns_limit_h_min              -11
_reflns_limit_k_max              35
_reflns_limit_k_min              -35
_reflns_limit_l_max              17
_reflns_limit_l_min              -18
_reflns_number_gt                5931
_reflns_number_total             6972
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ra03940h2.cif
_cod_data_source_block           2023uniandes_cu_05_pca-9_sq
_cod_original_sg_symbol_Hall     ' C -2yc'
_cod_database_code               7249357
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.79(3)
 0.21(3)
2. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 O8C-H8Ca = O8C-H8Cb
 0.85 with sigma of 0.02
 H8Ca-H8Cb
 1.34 with sigma of 0.04
 Zr3-H8Ca \\sim Zr3-H8Cb
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O16D) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O16D, O15D, O13D, S4D, O14D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O12D, O11D, O10D, O9D, S3D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4D, O1D, S1D, O2D, O3D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Rotating group:
 O7C(H7Ca,H7Cb), O6C(H6Ca,H6Cb), O5C(H5Ca,H5Cb), O4C(H4Ca,H4Cb), O2C(H2Ca,
 H2Cb), O3C(H3Ca,H3Cb), O1C(H1Ca,H1Cb)
6.b Ternary CH refined with riding coordinates:
 O1A(H1A), O2A(H2A), O4A(H4A), O3A(H3A)
6.c Me refined with riding coordinates:
 C8E(H8Ea,H8Eb,H8Ec), C6E(H6Ea,H6Eb,H6Ec), C4E(H4Ea,H4Eb,H4Ec)
6.d Idealised Me refined as rotating group:
 C2E(H2Ea,H2Eb,H2Ec)
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_smtbx_masks_special_details
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A solvent mask was calculated and 534 electrons were 
found in a volume of 1917\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 13[H2O] per Formula Unit 
which account for 520 electrons per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'