Compartmental ligand approach for constructing 3d–4f heterometallic [CuII5LnIII2] clusters: synthesis and magnetostructural properties
Jiang, Lin; Liu, Bin; Zhao, Hao-Wen; Tian, Jin-Lei; Liu, Xin; Yan, Shi-Ping; CrystEngComm 19 (2017) 1816–; doi:10.1039/C6CE02519F

data_7227737
_publ_section_title
;
 Compartmental ligand approach for constructing 3d--4f heterometallic
 [CuII5LnIII2] clusters: synthesis and magnetostructural properties
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1816
_journal_paper_doi               10.1039/C6CE02519F
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C46 H62 Cu5 N4 O22 Tm2, 2(N O3), 2(C2 H6 O)'
_chemical_formula_sum            'C50 H74 Cu5 N6 O30 Tm2'
_chemical_formula_weight         1894.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-02-14 deposited with the CCDC.
2017-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.605(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.8616(3)
_cell_length_b                   16.2208(4)
_cell_length_c                   18.8147(5)
_cell_measurement_reflns_used    4388
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7230
_cell_measurement_theta_min      2.9918
_cell_volume                     3798.39(17)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0716
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6696
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.760
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1878
_refine_diff_density_max         0.931
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6696
_refine_ls_number_restraints     449
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1290
_reflns_number_gt                4360
_reflns_number_total             6696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce02519f2.cif
_cod_data_source_block           0425-nk-jl-1_sq_d
_cod_depositor_comments
'Adding full bibliography for 7227732--7227739.cif.'
_cod_database_code               7227737
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C24-C25
 1.3 with sigma of 0.02
 C24-C25
 1.4 with sigma of 0.02
 C25-C24
 1.4 with sigma of 0.02
 C25-C24
 1.5 with sigma of 0.02
 H16-H19B
 1.9 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
5.a Ternary CH refined with riding coordinates:
 N1(H1), C10(H10), N2(H2)
5.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C11(H11A,H11B), C9(H9A,H9B), C8(H8A,H8B), C24(H24A,H24B)
5.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C5(H5), C14(H14), C16(H16), C4(H4), C6(H6A)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C)
5.e Idealised tetrahedral OH refined as rotating group:
 O15(H15A)
;
_olex2_submission_special_instructions 'No special instructions were received'