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_7227734
_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 Dy2 N4 O22, 2(C2 H5 O), 2(N O3), 4(C2 H6 O)'
_chemical_formula_sum            'C58 H96 Cu5 Dy2 N6 O34'
_chemical_formula_weight         2064.11
_chemical_name_systematic
;
 ? 
;
_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                 105.80(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.835(3)
_cell_length_b                   16.082(3)
_cell_length_c                   18.970(4)
_cell_measurement_reflns_used    5214
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4890
_cell_measurement_theta_min      3.5140
_cell_volume                     3767.7(15)
_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  0.0593
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13837
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.432
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2070
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.453
_refine_diff_density_min         -1.546
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         6631
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+12.0525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                5210
_reflns_number_total             6631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce02519f2.cif
_cod_data_source_block           cudy
_cod_depositor_comments
'Adding full bibliography for 7227732--7227739.cif.'
_cod_original_cell_volume        3767.6(13)
_cod_database_code               7227734
_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
 1.51 with sigma of 0.01
 O17-C25
 1.36 with sigma of 0.01
 O6-H6
 1 with sigma of 0.02
3. Rigid bond restraints
 O17, C25, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Ternary CH refined with riding coordinates:
 C10(H10), N1(H1), N2(H2)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C25(H25A,H25B),
 C28(H28A,H28B), C27(H27A,H27B)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6A), C4(H4), C15(H15), C14(H14), C16(H16)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C24(H24A,H24B,H24C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C29(H29A,H29B,H29C), C26(H26A,H26B,H26C)
4.e Idealised tetrahedral OH refined as rotating group:
 O15(H15A), O16(H16A)
;
_olex2_submission_special_instructions 'No special instructions were received'