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_7709236
_publ_section_title
;
 Self-assembly of non-macrocyclic triangular Ni<sub>3</sub>Ln clusters.
;
_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         'C38.5 H37.5 Ba N2 Ni3 O25, C H4 O, 2[CH4O]'
_chemical_formula_sum            'C41.5 H49.5 Ba N2 Ni3 O28'
_chemical_formula_weight         1337.80
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-19
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
;
2021-10-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                115.311(4)
_cell_angle_beta                 101.491(4)
_cell_angle_gamma                97.235(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0862(6)
_cell_length_b                   15.5290(9)
_cell_length_c                   16.8872(9)
_cell_measurement_reflns_used    9826
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      68.91
_cell_measurement_theta_min      3.24
_cell_volume                     2501.3(3)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0916
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            68110
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        65.082
_diffrn_reflns_theta_max         65.082
_diffrn_reflns_theta_min         3.017
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    8.148
_exptl_absorpt_correction_T_max  0.7539
_exptl_absorpt_correction_T_min  0.5561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1519 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.7376.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       block
_exptl_crystal_F_000             1353
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.202
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.00021(3)
_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   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         8413
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0711
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+37.2835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1625
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6808
_reflns_number_total             8413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03742k2.cif
_cod_data_source_block           tnd525h1
_cod_depositor_comments
'Adding full bibliography for 7709235--7709238.cif.'
_cod_original_formula_sum        'C41.50 H49.50 Ba N2 Ni3 O28'
_cod_database_code               7709236
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.356
_shelx_estimated_absorpt_t_min   0.279
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O16-H16
 0.87 with sigma of 0.01
 O1A-H1AA = O1A-H1AB
 0.84 with sigma of 0.01
 O1B-H1BA = O1B-H1BB
 0.84 with sigma of 0.01
 C62-H16
 1.878469 with sigma of 0.02
 Ni3-H16
 2.612313 with sigma of 0.02
 H1BA-H1BB
 1.33 with sigma of 0.02
 H1AA-H1AB
 1.33 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C62) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C61) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: H15A(0.5) H15B(0.5) C60(0.5) H60A(0.5) H60B(0.5) H60C(0.5)
 C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5)
5.a Free rotating group:
 O1A(H1AA,H1AB), O1B(H1BA,H1BB)
5.b Rotating group:
 O14(H14A,H14B), O17(H17A,H17B), O18(H18A,H18B), O15(H15A,H15B)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C26(H26), C27(H27), C29(H29), C12(H12), C9(H9), C52(H52), C32(H32),
 C7(H7), C8(H8), C46(H46), C28(H28), C6(H6), C51(H51), C31(H31), C47(H47),
 C48(H48), C49(H49)
5.d Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C60(H60A,H60B,H60C), C61(H61A,H61B,
 H61C), C63(H63A,H63B,H63C)
5.e Idealised tetrahedral OH refined as rotating group:
 O26(H26A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68724
_shelx_hkl_checksum              10071
_shelx_fab_checksum              9318
_olex2_submission_special_instructions 'No special instructions were received'