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_1565701
_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 N20 O12 Tm6, 6(Cl), 2(H2 O)'
_chemical_formula_sum            'C40 H116 Cl6 N20 O14 Tm6'
_chemical_formula_weight         2327.81
_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                 109.204(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.415(2)
_cell_length_b                   10.0407(11)
_cell_length_c                   22.500(3)
_cell_measurement_reflns_used    9142
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.006
_cell_measurement_theta_min      2.405
_cell_volume                     3715.4(8)
_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      293.15
_diffrn_measured_fraction_theta_full 0.998
_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  0.0834
_diffrn_reflns_av_unetI/netI     0.0693
_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       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30750
_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         2.786
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.366
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1547 before and 0.0700 after correction. The Ratio of minimum to maximum transmission is 0.6862. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.067
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.019
_refine_diff_density_max         1.408
_refine_diff_density_min         -1.340
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+14.2038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0869
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4996
_reflns_number_total             6590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-499-119201.cif
_cod_data_source_block           2g
_cod_original_cell_volume        3715.4(7)
_cod_database_code               1565701
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.638
_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. Others
 Fixed Sof: O2W(0.5) O3W(0.5)
3.a Ternary CH refined with riding coordinates:
 O1W(H1W), N1(H1), N3(H3), N5(H5), N7(H7), N9(H9)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B),
  C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), N2(H2C,H2D),
 N4(H4A,H4B), N6(H6C,H6D), N8(H8C,H8D), N10(H10C,H10D)
;