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_1565700
_publ_section_title
;
 A series of new polynuclear lanthanide(III) clusters prepared in alkylol
 amine
;
_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 Er6 N20 O12, 6(Cl), 2(H2 O)'
_chemical_formula_sum            'C40 H116 Cl6 Er6 N20 O14'
_chemical_formula_weight         2317.76
_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   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 108.948(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.4310(11)
_cell_length_b                   10.0145(7)
_cell_length_c                   22.5019(15)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.71
_cell_volume                     3715.1(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31481
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         3.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.979
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0660 before and 0.0516 after correction. The Ratio of minimum to maximum transmission is 0.8368. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_description       block
_exptl_crystal_F_000             2228
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.729
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         8469
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0160P)^2^+18.0648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0669
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6816
_reflns_number_total             8469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-499-119201.cif
_cod_data_source_block           2f
_cod_database_code               1565700
_shelx_estimated_absorpt_t_max   0.645
_shelx_estimated_absorpt_t_min   0.404
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups, All O(H) groups
2. Restrained distances
 N5-C11 = N6-C12
 1.46 with sigma of 0.01
 C11-C12
 1.51 with sigma of 0.01
 O3-C9 = O3-C9A
 1.42 with sigma of 0.02
 C9-C10 = C9A-C10A
 1.51 with sigma of 0.01
 N5-C10 = N5-C10A
 1.46 with sigma of 0.01
 H11A-H10F
 2.01 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 C11
\\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19
\\sim C20 \\sim C9 \\sim C9A \\sim C10 \\sim C10A: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C9) = Uanis(C9A)
Uanis(C10) = Uanis(C10A)
4. Others
 Sof(H5B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(H5A)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10C)=Sof(H10D)=FVAR(1)
 Fixed Sof: O2W(0.5) O3W(0.5)
5.a Ternary CH refined with riding coordinates:
 O1W(H1W), N1(H1), N3(H3), N5(H5A), N5(H5B), N7(H7), N9(H9)
5.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), N6(H6A,H6B), N8(H8A,H8B), N10(H10A,H10B), C1(H1A,
 H1B), C2(H2C,H2D), C3(H3A,H3B), C4(H4C,H4D), C5(H5C,H5D), C6(H6C,H6D), C7(H7A,
 H7B), C8(H8C,H8D), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
 C19(H19A,H19B), C20(H20A,H20B), C9(H9A,H9B), C9A(H9AA,H9AB), C10(H10C,H10D),
 C10A(H10E,H10F)
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