The role of 3d-4f exchange interaction in SMM behaviour and magnetic refrigeration of carbonato bridged CuLn (Ln = Dy, Tb and Gd) complexes of an unsymmetrical N<sub>2</sub>O<sub>4</sub> donor ligand.
Maity, Souvik; Mondal, Arpan; Konar, Sanjit; Ghosh, Ashutosh; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15170–15183; doi:10.1039/c9dt02627d

data_7701077
_publ_section_title
;
 The role of 3d-4f exchange interaction in SMM behaviour and magnetic
 refrigeration of carbonato bridged CuLn (Ln = Dy, Tb and Gd) complexes of
 an unsymmetrical N<sub>2</sub>O<sub>4</sub> donor ligand.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15170
_journal_page_last               15183
_journal_paper_doi               10.1039/c9dt02627d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C20 H22 Cu3 N2 O4, H2 O1, 2.5[H2O]'
_chemical_formula_sum            'C20 H29 Cu N2 O7.5'
_chemical_formula_weight         480.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-08-05
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.07.31 svn.r3643 for OlexSys, GUI svn.r5859)
;
_audit_update_record
;
2019-08-10 deposited with the CCDC.    2019-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                82.83(2)
_cell_angle_beta                 76.32(2)
_cell_angle_gamma                89.90(2)
_cell_formula_units_Z            6
_cell_length_a                   10.316(7)
_cell_length_b                   18.602(14)
_cell_length_c                   18.960(13)
_cell_measurement_reflns_used    72801
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.137
_cell_measurement_theta_min      2.208
_cell_volume                     3506(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1586
_diffrn_reflns_av_unetI/netI     0.1178
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            72729
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.208
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         12271
_refine_ls_number_restraints     715
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1666
_refine_ls_R_factor_gt           0.0860
_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^)+(0.0937P)^2^+7.0636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.2281
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6194
_reflns_number_total             12271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02627d2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'EMPIRICAL' changed to
'empirical' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7701077--7701080.cif.
;
_cod_original_formula_sum        'C20 H29 Cu N2 O7.50'
_cod_database_code               7701077
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.673
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C4A-C5A
 1.44 with sigma of 0.02
 C3A-C4A
 1.39 with sigma of 0.02
 C8AB-C9AB
 1.4 with sigma of 0.02
 C9AB-C10A
 1.42 with sigma of 0.02
 C20A-C19A \\sim C4-C3 \\sim C20C-C19C
 with sigma of 0.001
3. Rigid bond restraints
 C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C3 \\sim C4: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C9AB) \\sim Ueq, Uanis(C9AA) \\sim Ueq, Uanis(C8AB) \\sim Ueq,
Uanis(C8AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C16B, O4B, C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1A, C2A, C6A, O1A, C3A, O3A, C5A, C7A, Cu1A, C4A, C18A, N1A, N2A, O2A, C8AB,
 C10A, C11A, C17A, C9AB, C12A, C16A, C13A, C15A, O4A, C14A, C19A, C20A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1A, C8AA, C9AB, C10A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1A, C8AB, C9AA, C10A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N2B, C1B, C2B, C6B, O1B, C3B, O3B, C7B, C5B, Cu1B, C4B, C18B, N1B, O2B, C8B,
 C10B, C11B, C17B, C9B, C12B, C16B, C13B, C15B, O4B, C14B, C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1C, C2C, C6C, O1C, C3C, O3C, C5C, C7C, Cu1C, C4C, C18C, N1C, N2C, O2C, C8C,
 C10C, C11C, C17C, C9C, C12C, C16C, C13C, C15C, O4C, C14C, C19C, C20C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: C8AB(0.5) H8AA(0.5) H8AB(0.5) C9AB(0.5) H9AA(0.5) H9AB(0.5)
 H10A(0.5) H10B(0.5) H10C(0.5) H10D(0.5) C9AA(0.5) H9AC(0.5) H9AD(0.5)
 C8AA(0.5) H8AC(0.5) H8AD(0.5)
7.a Free rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB), O1(H1A,H1B)
7.b Secondary CH2 refined with riding coordinates:
 C8AB(H8AA,H8AB), C9AB(H9AA,H9AB), C10A(H10A,H10B), C10A(H10C,H10D), C19A(H19A,
 H19B), C8B(H8BA,H8BB), C9B(H9BA,H9BB), C10B(H10E,H10F), C8C(H8CA,H8CB),
 C9C(H9CA,H9CB), C10C(H10G,H10H), C19C(H19C,H19D), C3(H3C,H3D), C9AA(H9AC,H9AD),
  C8AA(H8AC,H8AD)
7.c Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C4A(H4A), C5A(H5A), C7A(H7A), C11A(H11A), C13A(H13A), C14A(H14A),
 C15A(H15A), C3B(H3B), C4B(H4B), C5B(H5B), C7B(H7B), C11B(H11B), C13B(H13B),
 C14B(H14B), C15B(H15B), C3C(H3CA), C4C(H4CA), C5C(H5C), C7C(H7C), C11C(H11C),
 C13C(H13C), C14C(H14C), C15C(H15C)
7.d Idealised Me refined as rotating group:
 C18A(H18A,H18B,H18C), C20A(H20A,H20B,H20C), C18B(H18D,H18E,H18F), C18C(H18G,
 H18H,H18I), C20C(H20D,H20E,H20F), C4(H4C,H4D,H4E)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 161 electrons were
found in a volume of 835\%A^3 in 1 void per unit cell.
This is consistent with the presence of 2.5[H2O] per
Formula Unit which account for 150 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              98116
_shelx_fab_checksum              6771
_olex2_submission_special_instructions 'No special instructions were received'