Structure-directing synthesis of two germanate cages featuring odd-member ring windows.
Li, Hao; Xu, Yanan; Zhang, Shiyue; Gu, Pengliang; Hu, Qing; Zhang, Yu; Wang, Wenkai; Shi, Zhan; Fu, Xinyi; Du, Hongbin; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13775–13782; doi:10.1039/d5dt01561h

data_7719300
_publ_section_title
;
 Structure-directing synthesis of two germanate cages featuring odd-member
 ring windows.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13775
_journal_page_last               13782
_journal_paper_doi               10.1039/d5dt01561h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'F2 Ge14 O32'
_chemical_formula_sum            'F2 Ge14 O32'
_chemical_formula_weight         1566.26
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.25505/fiz.icsd.cc2nwqcn
_audit_creation_date             2025-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-07-03 deposited with the CCDC.	2025-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   26.7307(11)
_cell_length_b                   26.7307(11)
_cell_length_c                   55.136(3)
_cell_measurement_reflns_used    5978
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      50.29
_cell_measurement_theta_min      2.88
_cell_volume                     34118(3)
_computing_cell_refinement       'SAINT V8.41 (?, 2016)'
_computing_data_collection       'APEX6 V2024.9-0 (Bruker, 2024)'
_computing_data_reduction        'SAINT V8.41 (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      193.0
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1487
_diffrn_reflns_av_unetI/netI     0.1259
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            67934
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        52.096
_diffrn_reflns_theta_max         52.096
_diffrn_reflns_theta_min         2.168
_diffrn_source                   MetalJet
_diffrn_source_current           3.57
_diffrn_source_power             0.2487933
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.384
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.6223
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1152 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.8284.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       block
_exptl_crystal_F_000             12996
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.151
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         12945
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1667
_refine_ls_R_factor_gt           0.0903
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1722P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2615
_refine_ls_wR_factor_ref         0.3135
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4456
_reflns_number_total             12945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01561h2.cif
_cod_data_source_block           6969_1_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7719300--7719301.cif.
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7719300
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.694
_shelx_estimated_absorpt_t_min   0.600
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU