More versatility than thought: large {Zr26} oxocarboxylate cluster by corner-sharing of standard octahedral subunits
Nateghi, Bahareh; Boldog, Ishtvan; Domasevitch, Konstiantyn V.; Janiak, Christoph; CrystEngComm 20 (2018) 5132–; doi:10.1039/C8CE01064A

data_7231381
_publ_section_title
;
 More versatility than thought: large {Zr26} oxocarboxylate cluster by
 corner-sharing of standard octahedral subunits
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              5132
_journal_paper_doi               10.1039/C8CE01064A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C35 H72 O123 Zr26, 5(C H2 O2) [+ solvent]'
_chemical_formula_sum            'C40 H82 O133 Zr26'
_chemical_formula_weight         5062.77
_chemical_name_systematic
'Henicosa-[\m~3~-oxido]-nonadeca-[\m~3~-hydroxido]-octa-[\m-hydroxido]-tetraicosa-[\m-formiato-\k^2^O1:O2]-tetra-[formiato-\k^2^O1:O2]-hepta-[formiato-\kO]-pentaaqua-hexaicosazirconium(IV) penta-formic acid solvate pentadecahydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-27 deposited with the CCDC.
2018-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                71.434(5)
_cell_angle_beta                 73.347(5)
_cell_angle_gamma                81.818(5)
_cell_formula_units_Z            1
_cell_length_a                   11.4132(8)
_cell_length_b                   18.7392(12)
_cell_length_c                   19.1989(11)
_cell_measurement_reflns_used    36620
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      70.953
_cell_measurement_theta_min      4.025
_cell_volume                     3723.3(4)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.127.0 (STOE, 2016)
;
_computing_data_reduction
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.77, Darmstadt 2016
;
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      ' 3195 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36620
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.953
_diffrn_reflns_theta_min         4.025
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    15.360
_exptl_absorpt_correction_T_max  0.6030
_exptl_absorpt_correction_T_min  0.4903
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.258
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2426
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.416
_refine_diff_density_min         -1.537
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         14209
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0561
_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^)+(0.1148P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1625
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10370
_reflns_number_total             14209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01064a2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7231381.cif.
;
_cod_database_code               7231381
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.579
_shelx_estimated_absorpt_t_max   0.749
_shelx_res_checksum              51273
_shelx_fab_checksum              43537