Unravelling the synthesis of a rare-earth cluster-based metal-organic framework with spn topology.
Bicalho, Hudson A.; Saraci, Felix; Velazquez-Garcia, Jose de J; Titi, Hatem M.; Howarth, Ashlee J.; Chemical communications (Cambridge, England) 58 (2022) 10925–10928; doi:10.1039/d2cc03575h

data_7130608
_publ_section_title
;
 Unravelling the synthesis of a rare-earth cluster-based metal-organic
 framework with spn topology.
;
_journal_issue                   78
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10925
_journal_page_last               10928
_journal_paper_doi               10.1039/d2cc03575h
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C360 H96 F128.001 O412.8 Y96'
_chemical_formula_sum            'C360 H96 F128 O412.8 Y96'
_chemical_formula_weight         21992.52
_chemical_name_common            Y-CU-45
_space_group_crystal_system      cubic
_space_group_IT_number           227
_space_group_name_Hall           '-F 4vw 2vw 3'
_space_group_name_H-M_alt        'F d -3 m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-05-18 deposited with the CCDC.	2022-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   36.079(4)
_cell_length_b                   36.079(4)
_cell_length_c                   36.079(4)
_cell_measurement_reflns_used    1173
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      22.618
_cell_measurement_theta_min      1.633
_cell_volume                     46964(9)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'High Precision 1-Axis Goniostat at P11 beamline(Petra III, DESY)'
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.61992
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            158966
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        21.836
_diffrn_reflns_theta_max         22.618
_diffrn_reflns_theta_min         1.633
_diffrn_source                   'undulator raditaion'
_exptl_absorpt_coefficient_mu    2.129
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             10454
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         2242
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0893P)^2^+69.5387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1313
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2004
_reflns_number_total             2242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03575h2.cif
_cod_data_source_block           y_cu_45
_cod_depositor_comments          'Adding full bibliography for 7130608.cif.'
_cod_original_cell_volume        46964(16)
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_original_formula_sum        'C360 H96 F128 O412.80 Y96'
_cod_database_code               7130608
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O3(0.15) C4(0.25) C5(0.125)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method MiTEGen
_olex2_submission_special_instructions 'No special instructions were received'