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_1565699
_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 Ho6 N20 O12, 6(Cl), 2(H2 O)'
_chemical_formula_sum            'C40 H116 Cl6 Ho6 N20 O14'
_chemical_formula_weight         2303.79
_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                 109.190(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.4640(10)
_cell_length_b                   10.0245(6)
_cell_length_c                   22.6388(15)
_cell_measurement_reflns_used    9188
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.136
_cell_measurement_theta_min      2.708
_cell_volume                     3743.1(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 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            82702
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.786
_exptl_absorpt_coefficient_mu    6.542
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0734 before and 0.0564 after correction. The Ratio of minimum to maximum transmission is 0.8885. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    2.040
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.039
_refine_diff_density_max         2.065
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         7355
_refine_ls_number_restraints     284
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0328P)^2^+23.5435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5937
_reflns_number_total             7355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-499-119201.cif
_cod_data_source_block           2e
_cod_database_code               1565699
_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 N(H,H,H,H)
  groups, All O(H) groups
2. Restrained distances
 C5A-C6A
 1.5 with sigma of 0.01
 C5-C6
 1.5 with sigma of 0.01
 C7-C8 = C7A-C8A
 1.51 with sigma of 0.01
 N3-C7 = N3-C7A = N4-C8 = N4-C8A
 1.46 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13
\\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C6
\\sim C6A \\sim C5 \\sim C5A \\sim C7 \\sim C7A \\sim C8 \\sim C8A: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(ClB)=1-FVAR(1)
 Sof(ClA)=FVAR(1)
 Sof(H3B)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=1-FVAR(2)
 Sof(H3A)=Sof(C6)=Sof(H6C)=Sof(H6D)=Sof(C5)=Sof(H5A)=Sof(H5B)=FVAR(2)
 Sof(H4BC)=Sof(H4BD)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 1-FVAR(3)
 Sof(H4AA)=Sof(H4AB)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8C)=Sof(H8D)=FVAR(3)
 Fixed Sof: O2W(0.5) O3W(0.5)
5.a Ternary CH refined with riding coordinates:
 O1W(H1W), N1(H1), N3(H3A), N3(H3B), N5(H5), N7(H7), N9(H9)
5.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4AA,H4AB), N4(H4BC,H4BD), N6(H6A,H6B), N8(H8A,H8B), N10(H10A,
 H10B), C1(H1A,H1B), C2(H2C,H2D), C3(H3C,H3D), C4(H4A,H4B), C9(H9A,H9B),
 C10(H10C,H10D), 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), C6(H6C,H6D), C6A(H6AA,H6AB), C5(H5A,H5B), C5A(H5AA,
 H5AB), C7(H7A,H7B), C7A(H7AA,H7AB), C8(H8C,H8D), C8A(H8AA,H8AB)
;