Heterospin 2p-4f and 2p-3d-4f complexes constructed by a nitronyl nitroxide ligand: syntheses, structures and magnetic properties
Sun, Juan; Chen, Min; Li, Ying; Liu, Xingran; Fu, Xinyang; He, Lijun; Jin, Chuan-Ming; CrystEngComm  (2022) –; doi:10.1039/D2CE01344D

data_7245761
_publ_section_title
;
 Heterospin 2p-4f and 2p-3d-4f complexes constructed by a nitronyl
 nitroxide ligand: syntheses, structures and magnetic properties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01344D
_journal_year                    2022
_chemical_formula_moiety         'C20 H4 F24 O8 Tb, C26 H23 Cu F6 N5 O4'
_chemical_formula_sum            'C46 H27 Cu F30 N5 O12 Tb'
_chemical_formula_weight         1634.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-23 deposited with the CCDC.	2022-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.342(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.054(2)
_cell_length_b                   20.134(2)
_cell_length_c                   17.469(2)
_cell_measurement_reflns_used    6257
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      3.2
_cell_volume                     5811.3(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57560
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_min         3.132
_exptl_absorpt_coefficient_mu    1.732
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         13253
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0372P)^2^+24.3262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8290
_reflns_number_total             13253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01344d2.cif
_cod_data_source_block           tbcu
_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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        5811.5(12)
_cod_database_code               7245761
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F30A) \\sim Ueq, Uanis(F30B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
3. Others
 Fixed Sof: F30A(0.5) F30B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C10(H10), C15(H15), C24(H24), C20(H20), C21(H21),
 C34(H34), C11(H11), C14(H14), C8(H8), C44(H44), C29(H29), C39(H39), C13(H13)
4.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C)
;
_olex2_submission_special_instructions 'No special instructions were received'