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_7718503
_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         'C20 H40 Cl2 Gd O5, C8 H16 Cl4 Gd O2'
_chemical_formula_structural     '[Gd(C4H8O)5Cl2][Gd(C4H8O)2Cl4]'
_chemical_formula_sum            'C28 H56 Cl6 Gd2 O7'
_chemical_formula_weight         1031.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-03-27 deposited with the CCDC.	2025-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.117(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   11.4240(10)
_cell_length_c                   26.624(2)
_cell_measurement_reflns_used    9012
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.13
_cell_measurement_theta_min      3.07
_cell_volume                     3812.9(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Diamond (H. Putz & K. Brandenburg, 2006, v. 4.6.4)'
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'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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            3536
_diffrn_reflns_point_group_measured_fraction_full 0.994
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.568
_diffrn_reflns_theta_min         3.567
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.908
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;    
SADABS-2014/5 - Bruker AXS area detector scaling and absorption
correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.113
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3536
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0212P)^2^+21.7400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3146
_reflns_number_total             3536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00254k2.cif
_cod_data_source_block           Gd-ionic
_cod_depositor_comments
'Adding full bibliography for 7718498--7718510.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7718503
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.519
_shelx_estimated_absorpt_t_max   0.666
_shelx_res_checksum              80116