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_7709238
_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         'C42 H42 Gd N2 Ni3 O24, 3(C H4 O), N O3'
_chemical_formula_sum            'C45 H54 Gd N3 Ni3 O30'
_chemical_formula_weight         1450.29
_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                 106.716(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0721(10)
_cell_length_b                   18.7861(11)
_cell_length_c                   17.1302(10)
_cell_measurement_reflns_used    9215
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      75.32
_cell_measurement_theta_min      3.58
_cell_volume                     5261.8(5)
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  Venture
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios Optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            143215
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         3.221
_diffrn_source                   'Bruker IuS DIAMOND'
_exptl_absorpt_coefficient_mu    10.111
_exptl_absorpt_correction_T_max  0.7540
_exptl_absorpt_correction_T_min  0.3595
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1629 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.4768.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_description       plate
_exptl_crystal_F_000             2932
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.000187(14)
_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   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         9641
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0232
_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^)+(0.0325P)^2^+4.7402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9335
_reflns_number_total             9641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03742k2.cif
_cod_data_source_block           ni3gd
_cod_depositor_comments
'Adding full bibliography for 7709235--7709238.cif.'
_cod_database_code               7709238
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.431
_shelx_estimated_absorpt_t_min   0.204
_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
2. Restrained distances
 O18-H18
 0.87 with sigma of 0.01
 O13-H13
 0.87 with sigma of 0.01
 O15-H15
 0.87 with sigma of 0.01
 O14-H14
 0.87 with sigma of 0.01
 O16-H16
 0.87 with sigma of 0.01
 Ni3-H16
 2.683098 with sigma of 0.02
 Ni4-H18
 2.693431 with sigma of 0.02
 C65-H18
 1.90243 with sigma of 0.02
 Ni3-H15
 2.622281 with sigma of 0.02
 C63-H16
 1.907772 with sigma of 0.02
 C60-H13
 1.906241 with sigma of 0.02
 Ni2-H13
 2.752081 with sigma of 0.02
 C62-H15
 1.912613 with sigma of 0.02
 C61-H14
 1.911506 with sigma of 0.02
 Ni2-H14
 2.702829 with sigma of 0.02
 N3B-O26B \\sim N3B-O27B \\sim N3B-O25B
 with sigma of 0.02
 O26B-O27B \\sim O27B-O25B \\sim O25B-O26B
 with sigma of 0.04
3. Restrained planarity
 N3B, O26B, O27B, O25B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N3B \\sim O26B \\sim O27B \\sim O25B: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N3A) \\sim Ueq, Uanis(O27A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 N3B, O26B, O27B, O25B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: N3B(0.65) O26B(0.65) O27B(0.65) O25B(0.65) O25A(0.35) N3A(0.35)
 O27A(0.35) O26A(0.35)
7.a Free rotating group:
 N3B(O26B,O27B,O25B)
7.b Aromatic/amide H refined with riding coordinates:
 C52(H52), C8(H8), C31(H31), C7(H7), C11(H11), C9(H9), C32(H32), C28(H28),
 C29(H29), C6(H6), C12(H12), C47(H47), C26(H26), C48(H48), C46(H46), C27(H27),
 C51(H51), C49(H49)
7.c Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C67(H67A,H67B,
 H67C), C64(H64A,H64B,H64C), C62(H62A,H62B,H62C), C65(H65A,H65B,H65C), C68(H68A,
 H68B,H68C), C66(H66A,H66B,H66C)
7.d Idealised tetrahedral OH refined as rotating group:
 O17(H17), O29(H29A), O30(H30), O28(H28A)
;
_shelx_res_checksum              37331
_shelx_hkl_checksum              1120
_olex2_submission_special_instructions 'No special instructions were received'