A series of new polynuclear lanthanide(III) clusters prepared in alkylol amine
Yang, Li-li; Zhou, Jian; Zou, Hua-Hong; Hu, Feilong; Zhao, Jun-Wei; Inorganica Chimica Acta 499 (2020) 119201–; doi:10.1016/j.ica.2019.119201

data_1565698
_publ_section_title
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 A series of new polynuclear lanthanide(III) clusters prepared in alkylol
 amine
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_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119201
_journal_paper_doi               10.1016/j.ica.2019.119201
_journal_volume                  499
_journal_year                    2020
_chemical_formula_moiety         'C40 H112 N20 O12 Tb6, 6(Cl), 2(H2 O)'
_chemical_formula_sum            'C40 H116 Cl6 N20 O14 Tb6'
_chemical_formula_weight         2267.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 108.637(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.4384(10)
_cell_length_b                   9.9388(5)
_cell_length_c                   22.5206(12)
_cell_measurement_reflns_used    8490
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.39
_cell_volume                     3698.5(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.098
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_min         2.717
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.940
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0773 before and 0.0515 after correction.
The Ratio of minimum to maximum transmission is 0.6568.
The \l/2 correction factor is Not present.
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_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.046
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.070
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         6579
_refine_ls_number_restraints     936
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+20.6950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5194
_reflns_number_total             6579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-499-119201.cif
_cod_data_source_block           2d
_cod_database_code               1565698
_shelx_estimated_absorpt_t_max   0.650
_shelx_estimated_absorpt_t_min   0.532
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups, All N(H,H)
  groups, All N(H,H,H,H) groups, All O(H) groups
2. Restrained distances
 N6-C11 = N6-C11A = C12-N5
 1.46 with sigma of 0.01
 C11-C12 = C11A-C12
 1.51 with sigma of 0.01
 O3-C9 = O3-C9A
 1.41 with sigma of 0.01
 C9-C10 = C9A-C10A
 1.5 with sigma of 0.01
 N5-C10 = N5-C10A
 1.46 with sigma of 0.01
 N5-H5
 0.98 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C13
\\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C12
\\sim C11 \\sim C11A \\sim C9 \\sim C9A \\sim C10 \\sim C10A \\sim N1 \\sim N2
\\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8 \\sim N9 \\sim N10 \\sim
O1W \\sim O1 \\sim O2 \\sim O2W \\sim O3 \\sim O3W \\sim O4 \\sim O5: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C13
\\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C12
\\sim C11 \\sim C11A \\sim C9 \\sim C9A \\sim C10 \\sim C10A: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H6BC)=Sof(H6BD)=Sof(H12C)=Sof(H12D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=1-FVAR(1)
 Sof(H6AA)=Sof(H6AB)=Sof(H12A)=Sof(H12B)=Sof(C11)=Sof(H11A)=Sof(H11B)=FVAR(1)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10E)=Sof(H10F)=1-FVAR(2)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10C)=Sof(H10D)=FVAR(2)
 Fixed Sof: O2W(0.5) O3W(0.5)
5.a Ternary CH refined with riding coordinates:
 O1W(H1W), N1(H1), N3(H3), N7(H7), N9(H9)
5.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), N6(H6AA,H6AB), N6(H6BC,H6BD), N8(H8A,H8B), N10(H10A,
 H10B), C1(H1A,H1B), C2(H2C,H2D), C3(H3A,H3B), C4(H4C,H4D), C5(H5A,H5B), C6(H6A,
 H6B), C7(H7A,H7B), C8(H8C,H8D), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
  C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,
 H20B), C12(H12A,H12B), C12(H12C,H12D), C11(H11A,H11B), C11A(H11C,H11D), C9(H9A,
 H9B), C9A(H9AA,H9AB), C10(H10C,H10D), C10A(H10E,H10F)
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