The effect of solvent molecules on crystallisation of heterotrinuclear MII–TbIII–MII complexes with tripodal nonadentate ligands
Takahara, Kazuma; Horino, Yuki; Wada, Koki; Sakata, Hiromu; Tomita, Daichi; Sunatsuki, Yukinari; Isobe, Hiroshi; Kojima, Masaaki; Suzuki, Takayoshi; CrystEngComm 26 (2024) 1004–1014; doi:10.1039/D3CE01192E

data_7247994
_publ_section_title
;
 The effect of solvent molecules on crystallisation of heterotrinuclear
 MII--TbIII--MII complexes with tripodal nonadentate ligands
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1004
_journal_page_last               1014
_journal_paper_doi               10.1039/D3CE01192E
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C61 H72 Mn2 N7 O18 Tb'
_chemical_formula_sum            'C61 H72 Mn2 N7 O18 Tb'
_chemical_formula_weight         1460.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2023-10-25 deposited with the CCDC.	2024-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.7164(8)
_cell_length_b                   15.9773(9)
_cell_length_c                   24.5892(12)
_cell_measurement_reflns_used    50458
_cell_measurement_temperature    188
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.00
_cell_volume                     6174.5(6)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2014 (Burla, et al., 2014)'
_diffrn_ambient_temperature      188
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            60028
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         3.005
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.611
_exptl_absorpt_correction_T_max  0.484
_exptl_absorpt_correction_T_min  0.205
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2984.00
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.650
_exptl_crystal_size_min          0.450
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.43
_refine_ls_abs_structure_details
;
 Flack x determined using 5852 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.424
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     805
_refine_ls_number_reflns         14086
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0194
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0680P)^2^+23.2334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0523
_reflns_Friedel_coverage         0.825
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                13606
_reflns_number_total             14086
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d3ce01192e2.cif
_cod_data_source_block           181205_boff2
_cod_depositor_comments
'Adding full bibliography for 7247989--7247998.cif.'
_cod_database_code               7247994
_shelx_res_checksum              93007