Solid State Structures and Solution Behaviour of Tetranuclear Lanthanide(III) Carbonate-Bridged Coordination Compounds of Chiral 3+3 Amine Macrocycle
Wydra, Karol Piotr; Kinzhybalo, Vasyl; Lisowski, Jerzy; Dalton Transactions  (2023) –; doi:10.1039/D3DT01948A

data_7713662
_publ_section_title
;
 Solid State Structures and Solution Behaviour of Tetranuclear
 Lanthanide(III) Carbonate-Bridged Coordination Compounds of Chiral 3+3
 Amine Macrocycle
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01948A
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'[Gd4, (C45 H64 N6 O3)2, (C O3)2, (N O3)2, (H2 O)4], (N O3)2, 9.7(C H4 O), 3.2(H2 O)'
_chemical_formula_sum            'C101.7 H181.2 Gd4 N16 O40.9'
_chemical_formula_weight         2911.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-07-28 deposited with the CCDC.	2023-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.33(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.967(4)
_cell_length_b                   16.817(3)
_cell_length_c                   19.356(4)
_cell_measurement_reflns_used    14462
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8450
_cell_measurement_theta_min      3.5640
_cell_volume                     6297(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25214
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.838
_diffrn_reflns_theta_min         3.306
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.164
_exptl_absorpt_correction_T_max  0.743
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             2973
_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.185
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 5747 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         14375
_refine_ls_number_restraints     621
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0297P)^2^+10.4707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0622
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.828
_reflns_number_gt                13286
_reflns_number_total             14375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01948a2.cif
_cod_data_source_block           wydrgd2a
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C101.70 H181.20 Gd4 N16 O40.90'
_cod_database_code               7713662
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.468
_shelx_estimated_absorpt_t_max   0.690
_shelx_res_checksum              71013