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_7709235
_publ_section_title
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 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
'C37 H34 La N2 Ni3 O25, C H4 O, 4(H2 O), N O3'
_chemical_formula_sum            'C38 H46 La N3 Ni3 O33'
_chemical_formula_weight         1387.82
_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
_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
;
2021-10-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.277(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4295(8)
_cell_length_b                   19.2819(15)
_cell_length_c                   24.0313(18)
_cell_measurement_reflns_used    9397
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      75.50
_cell_measurement_theta_min      2.97
_cell_volume                     4722.2(6)
_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
'PHOTON III M28 Charge-Integrating Pixel Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'Helios Optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28526
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         2.965
_diffrn_source                   'Bruker IuS DIAMOND'
_exptl_absorpt_coefficient_mu    9.197
_exptl_absorpt_correction_T_max  0.7540
_exptl_absorpt_correction_T_min  0.2310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1543 before and 0.0700 after correction.
The Ratio of minimum to maximum transmission is 0.3064.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_description       plate
_exptl_crystal_F_000             2800
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.915
_refine_diff_density_min         -2.268
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       0.00098(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   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         8337
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0580
_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^)+(0.1205P)^2^+11.9461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7886
_reflns_number_total             8337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03742k2.cif
_cod_data_source_block           tnd525h8
_cod_depositor_comments
'Adding full bibliography for 7709235--7709238.cif.'
_cod_database_code               7709235
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.710
_shelx_estimated_absorpt_t_min   0.216
_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
 O17-H17
 0.87 with sigma of 0.01
 Ni4-H17
 2.680886 with sigma of 0.02
 C60-H17
 1.89443 with sigma of 0.02
 La1-H25A \\sim La1-H25B
 with sigma of 0.02
3.a Free rotating group:
 O25(H25A,H25B), O33(H33A,H33B), O29(H29A,H29B), O30(H30A,H30B), O32(H32A,H32B)
3.b Rotating group:
 O16(H16A,H16B), O14(H14A,H14B), O15(H15A,H15B), O18(H18A,H18B), O13(H13A,H13B)
3.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C52(H52), C32(H32), C31(H31), C51(H51), C26(H26), C28(H28), C6(H6),
 C46(H46), C29(H29), C27(H27), C12(H12), C47(H47), C7(H7), C49(H49), C9(H9),
 C8(H8), C48(H48)
3.d Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C60(H60A,H60B,H60C)
3.e Idealised tetrahedral OH refined as rotating group:
 O31(H31A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91350
_shelx_hkl_checksum              52534
_olex2_submission_special_instructions 'No special instructions were received'