High-yield synthesis of heavy rare earth(III) anhydrous solvates: known, new, and unexpected products.
Barbosa, Guilherme A.; Carneiro Neto, José Severiano; Stoeberl, Bruno J.; Wisbeck, Sarita; Giese, Siddhartha O. K.; Yokaichiya, Fabiano; Costa, Daniel da S; Barison, Andersson; Ribeiro, Ronny R.; Piovan, Leandro; Hughes, David L.; Briganti, Matteo; Poneti, Giordano; Nunes, Giovana G.; Santana, Francielli S.; Soares, Jaísa F; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8251–8269; doi:10.1039/d5dt00254k

data_7718499
_publ_section_title
;
 High-yield synthesis of heavy rare earth(III) anhydrous solvates: known,
 new, and unexpected products.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8251
_journal_page_last               8269
_journal_paper_doi               10.1039/d5dt00254k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C8 H20 Cl3 Gd O4'
_chemical_formula_structural     '[Gd(C4H10O2)2Cl3]'
_chemical_formula_sum            'C8 H20 Cl3 Gd O4'
_chemical_formula_weight         443.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-03-12 deposited with the CCDC.	2025-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.716(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3944(8)
_cell_length_b                   8.8372(6)
_cell_length_c                   15.5800(11)
_cell_measurement_reflns_used    9791
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5610
_cell_measurement_theta_min      2.6721
_cell_volume                     1517.36(18)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection
'APEX4 v2022.10-0 - Bruker Instrument Service vV6.2.16'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics
'Diamond (H. Putz & K. Brandenburg, 2006, v. 4.6.4)'
_computing_publication_material
'SHELXL-2018/3 (Sheldrick, 2015) and WINGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0101
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            85683
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.497
_diffrn_reflns_theta_min         2.672
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.50
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.895
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.499
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.221
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.00315(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         5039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0140
_refine_ls_R_factor_gt           0.0118
_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^)+(0.0055P)^2^+0.9521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0235
_refine_ls_wR_factor_ref         0.0238
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4724
_reflns_number_total             5039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00254k2.cif
_cod_data_source_block           Gdglyme_new_synthesis
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' 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 7718498--7718510.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7718499
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              62656