Heterometallic Octanuclear Ni<sup>II</sup><sub>4</sub>Ln<sup>III</sup><sub>4</sub> (Ln = Y, Gd, Tb, Dy, Ho, Er) Complexes Containing Ni<sup>II</sup><sub>2</sub>Ln<sup>III</sup><sub>2</sub>O<sub>4</sub> Distorted Cubane Motifs: Synthesis, Structure, and Magnetic Properties.
Kalita, Pankaj; Goura, Joydeb; Herrera, Juan Manuel; Colacio, Enrique; Chandrasekhar, Vadapalli; ACS omega 3 (2018) 5202–5211; doi:10.1021/acsomega.8b00292

data_4515993
_publ_section_title
;
 Heterometallic Octanuclear
 Ni<sup>II</sup><sub>4</sub>Ln<sup>III</sup><sub>4</sub> (Ln = Y, Gd, Tb,
 Dy, Ho, Er) Complexes Containing
 Ni<sup>II</sup><sub>2</sub>Ln<sup>III</sup><sub>2</sub>O<sub>4</sub>
 Distorted Cubane Motifs: Synthesis, Structure, and Magnetic Properties.
;
_journal_issue                   5
_journal_name_full               'ACS omega'
_journal_page_first              5202
_journal_page_last               5211
_journal_paper_doi               10.1021/acsomega.8b00292
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C64 H98 Gd4 N8 Ni4 O34, 2(H O)'
_chemical_formula_sum            'C64 H100 Gd4 N8 Ni4 O36'
_chemical_formula_weight         2421.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-20
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.593(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8381(6)
_cell_length_b                   15.4317(6)
_cell_length_c                   23.4889(10)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.78
_cell_volume                     4622.7(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            70794
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.365
_diffrn_reflns_theta_min         1.582
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.704
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0909 before and 0.0606 after correction. The Ratio of minimum to maximum transmission is 0.7962. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.960
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         11505
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0496P)^2^+15.2722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9687
_reflns_number_total             11505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b00292_si_001.cif
_cod_data_source_block           ni4gd4
_cod_database_code               4515993
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.259
_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
 H1H-O1H
 0.84 with sigma of 0.002
 H1G-Gd2
 2.7 with sigma of 0.004
 H1H-O1H \\sim O2H-H2H \\sim H1G-O1G
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(O3B) = Uanis(O3A)
4.a Free rotating group:
 O1I(H1I)
4.b Ternary CH refined with riding coordinates:
 N2A(H2A), N2B(H2B)
4.c Secondary CH2 refined with riding coordinates:
 C8A(H8AA,H8AB), C8B(H8BA,H8BB), C9A(H9AA,H9AB), C9B(H9BA,H9BB), C10A(H10A,
 H10B), C10B(H10C,H10D), C11A(H11A,H11B), C11B(H11C,H11D)
4.d Aromatic/amide H refined with riding coordinates:
 C3A(H3AA), C3B(H3BA), C4A(H4A), C4B(H4B), C5A(H5A), C5B(H5B), C7A(H7A),
 C7B(H7B)
4.e Idealised Me refined as rotating group:
 C2C(H2CA,H2CB,H2CC), C2D(H2DA,H2DB,H2DC), C2E(H2EA,H2EB,H2EC), C2F(H2FA,H2FB,
 H2FC), C12A(H12A,H12B,H12C), C12B(H12D,H12E,H12F)
4.f Idealised tetrahedral OH refined as rotating group:
 O3A(H3A), O3B(H3B)
;
_shelx_res_checksum              19089
_shelx_hkl_checksum              71408
_shelx_fab_checksum              68189
_olex2_submission_special_instructions 'No special instructions were received'