Self-assembled octanuclear [Ni<sub>5</sub>Ln<sub>3</sub>] (Ln = Dy, Tb and Ho) complexes: synthesis, coordination induced ligand hydrolysis, structure and magnetism.
Bhanja, Avik; Moreno-Pineda, Eufemio; Herchel, Radovan; Wernsdorfer, Wolfgang; Ray, Debashis; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7968–7976; doi:10.1039/d0dt01675f

data_7704421
_publ_section_title
;
 Self-assembled octanuclear [Ni<sub>5</sub>Ln<sub>3</sub>] (Ln = Dy, Tb
 and Ho) complexes: synthesis, coordination induced ligand hydrolysis,
 structure and magnetism.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7968
_journal_page_last               7976
_journal_paper_doi               10.1039/d0dt01675f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C80 H94 N4 Ni5 O36 Tb3, 7(H2O),(NO3)'
_chemical_formula_sum            'C80 H108 N5 Ni5 O46 Tb3'
_chemical_formula_weight         2627.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-03-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-05-08 deposited with the CCDC.	2020-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.094(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.194(3)
_cell_length_b                   23.629(3)
_cell_length_c                   20.418(3)
_cell_measurement_reflns_used    7615
_cell_measurement_temperature    114.51
_cell_measurement_theta_max      25.061
_cell_measurement_theta_min      2.286
_cell_volume                     10647(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       SMART
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      114.51
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX-II'
_diffrn_measurement_method       'CCD area detector, \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.0766
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42297
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.061
_diffrn_reflns_theta_max         25.061
_diffrn_reflns_theta_min         2.526
_exptl_absorpt_coefficient_mu    2.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            'Pale green'
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       Needle'
_exptl_crystal_F_000             5352
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   0.747
_exptl_transmission_factor_min   0.663
_refine_diff_density_max         3.054
_refine_diff_density_min         -2.012
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         9397
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0662
_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^)+(0.1311P)^2^+55.2698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.1970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7615
_reflns_number_total             9397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01675f2.cif
_cod_data_source_block           Complex2
_cod_depositor_comments
'Adding full bibliography for 7704420--7704422.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C80 H108 Tb3 N5 Ni5 O46'
_cod_database_code               7704421
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C22-C21 = C22-C21A = C21A-C20A = C21-C20 = C20A-C19A = C20-C19 = C19A-C18 =
 C19-C18 = C23-C18
 1.39 with sigma of 0.02
 O2N-N1N = O3N-N1N = O4N-N1N
 1.24 with sigma of 0.02
 O12-H12
 0.85 with sigma of 0.02
 O15-H15
 0.85 with sigma of 0.02
 O14-H14
 0.85 with sigma of 0.02
 O13-H13
 0.85 with sigma of 0.02
 H17A-O17
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C19 \\sim C20 \\sim C21 \\sim C19A \\sim C20A \\sim C21A: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
O2N \\sim O3N \\sim O4N \\sim N1N: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 1.7A
4. Others
 Fixed Sof: C19(0.5) H19(0.5) C20(0.5) H20(0.5) C21(0.5) H21(0.5) C19A(0.5)
 H19A(0.5) C20A(0.5) H20A(0.5) C21A(0.5) H21A(0.5) O2N(0.5) O3N(0.5) O4N(0.5)
 N1N(0.5) O5W(0.5)
5.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
5.b Rotating group:
 O16(H16A,H16B), O18(H18A,H18B)
5.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C25(H25A,H25B)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C12(H12A), C13(H13A), C19(H19),
 C20(H20), C21(H21), C24(H24), C27(H27), C28(H28), C29(H29), C35(H35), C36(H36),
  C37(H37), C40(H40), C19A(H19A), C20A(H20A), C21A(H21A)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16C,H16D,H16E), C17(H17C,H17D,H17E), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              73110
_shelx_fab_checksum              63188
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'