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_7706821
_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         'C65 H79 Gd2 N4 Ni6 O30, 8 H2O'
_chemical_formula_sum            'C65 H95 Gd2 N4 Ni6 O38'
_chemical_formula_weight         2207.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-01-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-27 deposited with the CCDC.	2021-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                113.93(2)
_cell_angle_beta                 103.87(6)
_cell_angle_gamma                102.08(5)
_cell_formula_units_Z            1
_cell_length_a                   11.53(2)
_cell_length_b                   14.72(2)
_cell_length_c                   15.378(19)
_cell_measurement_reflns_used    5607
_cell_measurement_temperature    114(2)
_cell_measurement_theta_max      26.482
_cell_measurement_theta_min      2.518
_cell_volume                     2174(6)
_computing_cell_refinement       'SHELXL 2014/5 (Sheldrick, 2014)'
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      114.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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  0.0585
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34276
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.482
_diffrn_reflns_theta_min         2.518
_exptl_absorpt_coefficient_mu    2.846
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_correction_T_min  0.584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       needle
_exptl_crystal_F_000             1033
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.211
_refine_diff_density_min         -1.677
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8932
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+8.0585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5607
_reflns_number_total             8932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04168h2.cif
_cod_data_source_block           complex1
_cod_depositor_comments
'Adding full bibliography for 7706821--7706822.cif.'
_cod_database_code               7706821
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.745
_shelx_estimated_absorpt_t_min   0.561
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H11 of O11, H10 of O10, H8 of O8, H9 of O9, All C(H,H)
  groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H14C of O14
2. Restrained distances
 O14-C33
 1.45 with sigma of 0.05
 C31-O13 \\sim C31A-O13A
 with sigma of 0.02
 C31-O12 \\sim C31A-O12A
 with sigma of 0.02
 C31-C32 \\sim C31A-C32A
 with sigma of 0.02
 Ni1-O14 \\sim Ni1-O14A
 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
O13 \\sim O13A \\sim O12 \\sim O12A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C32 \\sim C32A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C31 \\sim C31A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(O14) = Uanis(O14A)
4. Rigid body (RIGU) restrains
 C33, O14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31A, C32A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O13(0.5) O12(0.5) H16B(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5)
 O14A(0.5) H14A(0.5) H14B(0.5) O14(0.5) H14C(0.5) C31(0.5) C31A(0.5) O13A(0.5)
 O12A(0.5) C32A(0.5) H32D(0.5) H32E(0.5) H32F(0.5) C33(0.5) H33A(0.5) H33B(0.5)
 H33C(0.5)
6.a Ternary CH refined with riding coordinates:
 O11(H11), O9(H9), O8(H8)
6.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C8(H8A,H8B), O7(H7A,H7B)
6.c Me refined with riding coordinates:
 C32(H32A,H32B,H32C), C32A(H32D,H32E,H32F)
6.d Aromatic/amide H refined with riding coordinates:
 O10(H10), C14(H14), C20(H20), C9(H9A), C13(H13), C24(H24), C3(H3), C26(H26),
 C19(H19), C5(H5), C18(H18), C27(H27), C12(H12), C29(H29), C11(H11A), C34(H34),
 C28(H28)
6.e Tetrahedral OH refined with riding coordinates:
 O14(H14C)
6.f X=CH2 refined with riding coordinates:
 O15(H15A,H15B), O14A(H14A,H14B)
6.g Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              62357
_shelx_fab_checksum              57668
_olex2_submission_special_instructions 'No special instructions were received'