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_7713665
_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]0.5, [Gd4, (C45 H63 N6 O3)2, (C O3)2, (N O3)2, (H2 O)4]0.5, (N O3), 6.38(C H4 O), 6.7(H2 O)'
_chemical_formula_sum            'C98.38 H173.92 Gd4 N15 O38.08'
_chemical_formula_weight         2805.27
_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                 103.91(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.134(5)
_cell_length_b                   16.859(4)
_cell_length_c                   19.337(5)
_cell_measurement_reflns_used    67113
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.6250
_cell_measurement_theta_min      2.3430
_cell_volume                     6371(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            107537
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         75.738
_diffrn_reflns_theta_min         2.354
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.910
_exptl_absorpt_correction_T_max  0.445
_exptl_absorpt_correction_T_min  0.067
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             2860
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.139
_refine_diff_density_max         1.083
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Flack x determined using 5077 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     843
_refine_ls_number_reflns         12557
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+18.8747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.841
_reflns_Friedel_fraction_full    0.945
_reflns_Friedel_fraction_max     0.895
_reflns_number_gt                12130
_reflns_number_total             12557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01948a2.cif
_cod_data_source_block           wydrgd1ab
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7713665
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.109
_shelx_estimated_absorpt_t_max   0.248
_shelx_res_checksum              14279