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_7704420
_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 Dy3 N4 Ni5 O36, 7(H2O), NO3'
_chemical_formula_sum            'C80 H108 Dy3 N5 Ni5 O46'
_chemical_formula_weight         2656.69
_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                 96.071(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.13(3)
_cell_length_b                   23.55(4)
_cell_length_c                   20.35(3)
_cell_measurement_reflns_used    7375
_cell_measurement_temperature    114(2)
_cell_measurement_theta_max      26.596
_cell_measurement_theta_min      1.556
_cell_volume                     10546(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      114.51
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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  0.0903
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67366
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.596
_diffrn_reflns_theta_min         1.556
_exptl_absorpt_coefficient_mu    3.061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            'Pale green'
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       Needle
_exptl_crystal_F_000             5396
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   0.714
_exptl_transmission_factor_min   0.582
_refine_diff_density_max         1.131
_refine_diff_density_min         -1.270
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         10913
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+12.1516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7375
_reflns_number_total             10913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01675f2.cif
_cod_data_source_block           Complex1
_cod_depositor_comments
'Adding full bibliography for 7704420--7704422.cif.'
_cod_original_cell_volume        10545(27)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7704420
_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
 O4N-N1N = O2N-N1N = O3N-N1N
 1.24 with sigma of 0.01
 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
 O18-H18B = O18-H18A
 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 0.01 and sigma for terminal atoms of 0.02 within 1.7A
O2N \\sim O3N \\sim O4N \\sim N1N: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 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) O5W(0.5) O2N(0.5) O3N(0.5)
 O4N(0.5) N1N(0.5)
5.a Rotating group:
 O16(H16A,H16B), O17(H17A,H17B)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C25(H25A,H25B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C12(H12A), C13(H13A), C24(H24),
 C27(H27), C28(H28), C29(H29), C35(H35), C36(H36), C37(H37), C40(H40), C19(H19),
  C20(H20), C21(H21), C19A(H19A), C20A(H20A), C21A(H21A)
5.d 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              64401
_shelx_fab_checksum              61063
_olex2_submission_special_instructions 'No special instructions were received'