Diacylhydrazone-assembled {Ln<sub>11</sub>} nanoclusters featuring a "double-boats conformation" topology: synthesis, structures and magnetism.
Wang, Kai; Chen, Zi-Lu; Zou, Hua-Hong; Zhang, Shu-Hua; Li, Yan; Zhang, Xiu-Qing; Sun, Wei-Yin; Liang, Fu-Pei; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2337–2343; doi:10.1039/c7dt03179c

data_7045265
_publ_section_title
;
 Diacylhydrazone-assembled {Ln<sub>11</sub>} nanoclusters featuring a
 &quot;double-boats conformation&quot; topology: synthesis, structures and
 magnetism.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2337
_journal_page_last               2343
_journal_paper_doi               10.1039/c7dt03179c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C98 H98 N28 O68 Tb11, 0.5(H6 O4), 3(C H4 O)'
_chemical_formula_sum            'C101 H112.99 N28 O73 Tb11'
_chemical_formula_weight         4635.30
_chemical_name_systematic        'SuperNova, Single source at offset'
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-12 deposited with the CCDC.
2018-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.6758(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.3869(5)
_cell_length_b                   12.88765(16)
_cell_length_c                   33.2931(4)
_cell_measurement_reflns_used    27144
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      28.8185
_cell_measurement_theta_min      2.8659
_cell_volume                     13422.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            66443
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.872
_exptl_absorpt_coefficient_mu    5.828
_exptl_absorpt_correction_T_max  0.5934
_exptl_absorpt_correction_T_min  0.5180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.294
_exptl_crystal_description       block
_exptl_crystal_F_000             8856
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.268
_refine_diff_density_min         -5.468
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         13156
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0519P)^2^+488.1417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10794
_reflns_number_total             13156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03179c2.cif
_cod_data_source_block           2-Tb11
_cod_depositor_comments
'Adding full bibliography for 7045264--7045266.cif.'
_cod_database_code               7045265
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.593
_shelx_estimated_absorpt_t_min   0.518
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1WA,H1WB} of O1W, H35A of O35, H20 of O20, H21 of O21,
  H15 of O15, H16 of O16, H19A of O19, H17 of O17
 At 1.5 times of:
  All C(H,H,H) groups, H3W of O3W, {H2WA,H2WB} of O2W
2. Restrained distances
 O20-C56
 1.4 with sigma of 0.01
 O22-C55
 1.1 with sigma of 0.01
 Tb2-O20
 2.6 with sigma of 0.01
 O19-C57
 1.4 with sigma of 0.01
 N13-O30 = N13-O29 = N13-O31 = N13-O30'
 1.2 with sigma of 0.02
 O30-O29 = O30-O31 = O29-O31
 2.4 with sigma of 0.02
 O30'-O29 = O30'-O31
 2.4 with sigma of 0.02
3. Rigid bond restraints
 Tb2, O20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O22, C55
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O30, N13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O20 \\sim C56 \\sim O2W: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(C57)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O29) \\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O20)
\\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N13) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(O35) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Others
 Fixed Sof: Tb5(0.5) Tb5'(0.5) O3W(0.5) H3W(0.5) O19(0.5) H19A(0.5) O30(0.5)
 O30'(0.5) N1(0.5) N1'(0.5) N2(0.5) N2'(0.5) C57(0.5) H57A(0.5) H57B(0.5)
 H57C(0.5) O2W(0.5) H2WA(0.5) H2WB(0.5)
6.a Everything fixed:
 O20, O29, O30, O30', O31, N13, C55, C56
6.b Fixed occupancy and ADP/Uiso:
 O11
6.c Riding coordinates:
 O1W(H1WA,H1WB), O3W(H3W), O15(H15), O16(H16), O17(H17), O19(H19A), O20(H20),
 O21(H21), C1(H1A,H1B,H1C), C3(H3), C5(H5), C11(H11), C12(H12), C13(H13),
 C16(H16A), C18(H18), C19(H19), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C27(H27), C28(H28), C31(H31), C34(H34), C35(H35), C36(H36), C39(H39), C41(H41),
  C42(H42), C43(H43), C46(H46A,H46B,H46C), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), O2W(H2WA,H2WB), O35(H35A), C51(H51A,H51B,H51C)
6.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C26(H26)
6.e Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C)
;
_shelx_res_checksum              95286