Hydroxido supported and differently networked octanuclear Ni<sub>6</sub>Ln<sub>2</sub> [Ln = Gd<sup>III</sup> and Dy<sup>III</sup>] complexes: structural variation, magnetic properties and theoretical insights.
Bhanja, Avik; Smythe, Lucy; Herchel, Radovan; Nemec, Ivan; Murrie, Mark; Ray, Debashis; Dalton transactions (Cambridge, England : 2003) 50 (2021) 5023–5035; doi:10.1039/d0dt04168h

data_7706822
_publ_section_title
;
 Hydroxido supported and differently networked octanuclear
 Ni<sub>6</sub>Ln<sub>2</sub> [Ln = Gd<sup>III</sup> and Dy<sup>III</sup>]
 complexes: structural variation, magnetic properties and theoretical
 insights.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5023
_journal_page_last               5035
_journal_paper_doi               10.1039/d0dt04168h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C61.2 H66.4 Cl5.2 Dy2 N4 Ni5.6 O20, 2(CH3OH), 4[H2O]'
_chemical_formula_sum            'C63.2 H82.4 Cl5.2 Dy2 N4 Ni5.6 O26'
_chemical_formula_weight         2152.29
_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             2021-03-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-05 deposited with the CCDC.	2021-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.55(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.705(6)
_cell_length_b                   13.771(3)
_cell_length_c                   23.455(5)
_cell_measurement_reflns_used    5685
_cell_measurement_temperature    112.15
_cell_measurement_theta_max      25.150
_cell_measurement_theta_min      1.629
_cell_volume                     8074(4)
_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 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      112.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART APEX-III'
_diffrn_measurement_method       'CCD area detector,\w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47149
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.150
_diffrn_reflns_theta_max         25.150
_diffrn_reflns_theta_min         1.629
_exptl_absorpt_coefficient_mu    3.343
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       block
_exptl_crystal_F_000             4139
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.337
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         7168
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0578P)^2^+73.9082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1257
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5685
_reflns_number_total             7168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04168h2.cif
_cod_data_source_block           complex2
_cod_depositor_comments
'Adding full bibliography for 7706821--7706822.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C63.20 H82.40 Cl5.20 Dy2 N4 Ni5.60 O26'
_cod_database_code               7706822
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.690
_shelx_estimated_absorpt_t_min   0.617
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H7 of O7, H9A of O9A, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H11A of O11, H11B of O11A, H8 of O8, All O(H,H) groups
2. Restrained distances
 O11A-C32A
 1.44 with sigma of 0.02
 C32-O11 \\sim C32A-O11A
 with sigma of 0.02
 Dy1-H10A \\sim Dy1-H10B
 with sigma of 0.02
 Ni1-H9BA \\sim Ni1-H9BB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O9A) \\sim Ueq, Uanis(O9B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O11) = Uanis(O11A)
Uanis(C32) = Uanis(C32A)
Uanis(O9A) = Uanis(O9B)
Uanis(Cl1) = Uanis(Cl1A)
4. Others
 Sof(O11A)=Sof(H11B)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(1)
 Sof(O11)=Sof(H11A)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
 Fixed Sof: Ni3(0.8) Cl1(0.8) Cl2(0.8) Cl3(0.8) O9A(0.6) H9A(0.6) O9B(0.4)
 H9BA(0.4) H9BB(0.4) C31(0.6) H31A(0.6) H31B(0.6) H31C(0.6) Cl1A(0.2)
5.a Riding coordinates:
 O9B(H9BA,H9BB)
5.b Free rotating group:
 O10(H10A,H10B)
5.c Ternary CH refined with riding coordinates:
 O7(H7), O8(H8)
5.d Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C8(H8A,H8B)
5.e Aromatic/amide H refined with riding coordinates:
 O9A(H9A), C9(H9), C29(H29), C18(H18), C24(H24), C20(H20), C14(H14), C3(H3),
 C4(H4), C26(H26), C19(H19), C11(H11), C5(H5), C13(H13), C27(H27), C12(H12),
 C28(H28)
5.f Tetrahedral OH refined with riding coordinates:
 O11(H11A), O11A(H11B)
5.g Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C1(H1A,H1B,H1C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C32A(H32D,H32E,H32F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 176 electrons were 
found in a volume of 1088\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[2H2O] per Asymmetric Unit 
which account for 136 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99363
_shelx_fab_checksum              4784
_olex2_submission_special_instructions 'No special instructions were received'