Self-assembly of non-macrocyclic triangular Ni<sub>3</sub>Ln clusters.
Dais, Tyson N.; Takano, Rina; Ishida, Takayuki; Plieger, Paul G.; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1446–1453; doi:10.1039/d1dt03742k

data_7709237
_publ_section_title
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 Self-assembly of non-macrocyclic triangular Ni<sub>3</sub>Ln clusters.
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_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1446
_journal_page_last               1453
_journal_paper_doi               10.1039/d1dt03742k
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C36 H30 Eu N2 Ni3 O24, N O3, 1.5(C H4 O)'
_chemical_formula_sum            'C37.5 H36 Eu N3 Ni3 O28.5'
_chemical_formula_weight         1312.78
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-10-18
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
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2021-10-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.203(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.7986(12)
_cell_length_b                   16.5467(16)
_cell_length_c                   39.972(4)
_cell_measurement_reflns_used    9720
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      75.66
_cell_measurement_theta_min      4.50
_cell_volume                     8465.0(14)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Image Plate'
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  Venture
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            129662
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.231
_diffrn_reflns_theta_min         2.211
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    12.934
_exptl_absorpt_correction_T_max  0.7540
_exptl_absorpt_correction_T_min  0.3986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1470 before and 0.0690 after correction.
The Ratio of minimum to maximum transmission is 0.5286.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.060
_exptl_crystal_description       block
_exptl_crystal_F_000             5256
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.000172(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         7697
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0424P)^2^+19.8887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7657
_reflns_number_total             7697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03742k2.cif
_cod_data_source_block           tnd525h4
_cod_depositor_comments
'Adding full bibliography for 7709235--7709238.cif.'
_cod_original_cell_volume        8464.9(14)
_cod_original_formula_sum        'C37.50 H36 Eu N3 Ni3 O28.50'
_cod_database_code               7709237
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H29A of O29
 At 1.5 times of:
  All C(H,H,H) groups, H28A of O28, All O(H,H) groups
2. Restrained distances
 Ni3-H16A \\sim Ni3-H16B
 with sigma of 0.02
 Ni3-H15A \\sim Ni3-H15B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C60) \\sim Ueq, Uanis(O28) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Fixed Sof: O29(0.5) H29A(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5)
5.a Free rotating group:
 O16(H16A,H16B), O15(H15A,H15B)
5.b Rotating group:
 O13(H13A,H13B), O18(H18A,H18B), O17(H17A,H17B), O14(H14A,H14B), O29(H29A)
5.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C32(H32), C51(H51), C31(H31), C52(H52), C12(H12), C26(H26), C11(H11),
 C29(H29), C8(H8), C46(H46), C28(H28), C7(H7), C49(H49), C6(H6), C47(H47),
 C48(H48), C27(H27)
5.d Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C)
5.e Idealised tetrahedral OH refined as rotating group:
 O28(H28A)
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_shelx_res_checksum              50719
_shelx_hkl_checksum              25847
_olex2_submission_special_instructions 'No special instructions were received'