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_7045264
_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 Gd11 N28 O68, H2 O, H O, 3(C H4 O)'
_chemical_formula_sum            'C101 H113 Gd11 N28 O73'
_chemical_formula_weight         4616.94
_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             2017-12-11
_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                 94.857(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.361(4)
_cell_length_b                   12.9403(15)
_cell_length_c                   33.405(4)
_cell_measurement_reflns_used    58212
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      1.22
_cell_volume                     13508(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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0682
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            52765
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         1.703
_exptl_absorpt_coefficient_mu    5.433
_exptl_absorpt_correction_T_max  0.6127
_exptl_absorpt_correction_T_min  0.5618
_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    2.270
_exptl_crystal_description       block
_exptl_crystal_F_000             8812
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.709
_refine_diff_density_min         -3.278
_refine_diff_density_rms         0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         11677
_refine_ls_number_restraints     382
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0781
_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^+1647.9542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1824
_refine_ls_wR_factor_ref         0.1910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9875
_reflns_number_total             11677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03179c2.cif
_cod_data_source_block           1-Gd11
_cod_depositor_comments
'Adding full bibliography for 7045264--7045266.cif.'
_cod_database_code               7045264
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.613
_shelx_estimated_absorpt_t_min   0.562
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H35A of O35, H19A of O19, H17 of O17, H20 of O20, H15 of
  O15, H21 of O21, H16 of O16
 At 1.5 times of:
  All C(H,H,H) groups, H3W of O3W, All O(H,H) groups
2. Restrained distances
 O20-C56
 1.4 with sigma of 0.01
 O22-C55
 1.1 with sigma of 0.01
 Gd2-O20
 2.6 with sigma of 0.01
 N13-O30 = N13-O29 = N13-O31 = N13-O30'
 1.2 with sigma of 0.02
 O30'-O29 = O30'-O31
 2.4 with sigma of 0.02
 H35A-H51C
 2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Gd2 \\sim O20 \\sim C56: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Gd4 \\sim O17 \\sim O26 \\sim O28 \\sim N12: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Gd5' \\sim O32 \\sim O33 \\sim O34 \\sim N14: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.01
Gd4 \\sim O29 \\sim O30 \\sim O30' \\sim O31: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.01
O1 \\sim O1W \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8
\\sim O9 \\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16
\\sim O17 \\sim O18 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25
\\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O30' \\sim O31 \\sim
O32 \\sim O33 \\sim O34 \\sim O2W \\sim O3W \\sim O19 \\sim O35: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
Gd1 \\sim O22 \\sim O23 \\sim O24 \\sim N1: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(O3W) \\sim Ueq, Uanis(C38)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(O7)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N6) \\sim Ueq,
Uanis(N7) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(O16) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2) \\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(O28)
\\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O30') \\sim Ueq, Uanis(N13) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(O14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: Gd5(0.5) Gd5'(0.5) O30(0.5) O30'(0.5) O2W(0.5) H2WA(0.5) H2WB(0.5)
 O3W(0.5) H3W(0.5) O19(0.5) H19A(0.5) C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5)
5.a Everything fixed:
 O25, O26, C55, O2W
5.b Fixed occupancy and ADP/Uiso:
 O7, O8, O11, O14, N8, C15
5.c Riding coordinates:
 O1W(H1WA,H1WB), O15(H15), O16(H16), O17(H17), O20(H20), O21(H21), C1(H1A,H1B,
 H1C), C3(H3), C5(H5), C8(H8), C11(H11), C12(H12), C13(H13), C18(H18), C19(H19),
  C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26), C27(H27), C28(H28),
 C31(H31), C34(H34), C35(H35), C36(H36), C39(H39), C41(H41), C42(H42), C43(H43),
  C46(H46A,H46B,H46C), C49(H49A,H49B,H49C), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C), O2W(H2WA,H2WB), O3W(H3W), O19(H19A), C57(H57A,H57B,H57C), O35(H35A),
 C51(H51A,H51B,H51C)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C16(H16A)
;
_shelx_res_checksum              74501