A series of six-member lanthanide-rings based on 2,2-bis(hydroxymethyl)-2,2’,2’’-nitrilotriethanol : synthesis, crystal structures and magnetic properties
li, bao; hu, peng; yin, lei; Mao, Nannan; Yu, Fan; Wang, Zhenxing; Zhang, Tianle; CrystEngComm  (2017) –; doi:10.1039/C7CE01063J

data_7228692
_publ_section_title
;
 A series of six-member lanthanide-rings based on
 2,2-bis(hydroxymethyl)-2,2&#x2019;,2&#x2019;&#x2019;-nitrilotriethanol :
 synthesis, crystal structures and magnetic properties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01063J
_journal_year                    2017
_chemical_formula_moiety         'C90 H132 N6 O42 Tb6,2(H2 O),C7 H8'
_chemical_formula_sum            'C97 H144 N6 O44 Tb6'
_chemical_formula_weight         3051.74
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc1nv7rh
_audit_creation_date             2017-07-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.06.29 svn.r3433 for OlexSys, GUI svn.r5356)
;
_audit_update_record
;
2017-07-14 deposited with the CCDC.
2017-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   26.742(4)
_cell_length_b                   26.742(4)
_cell_length_c                   78.391(16)
_cell_measurement_reflns_used    25920
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.000
_cell_measurement_theta_min      0.917
_cell_volume                     48549(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0341
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_number            21200
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         0.917
_exptl_absorpt_coefficient_mu    3.967
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_description       block
_exptl_crystal_F_000             25920
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The disordered solvent molecules are a mixture of two
H2O and one toulene for each hexanuclear ring.
;
_refine_diff_density_max         3.182
_refine_diff_density_min         -1.305
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1331
_refine_ls_number_reflns         21200
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+399.0363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18469
_reflns_number_total             21200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01063j2.cif
_cod_data_source_block           2
_cod_original_cell_volume        48548(17)
_cod_database_code               7228692
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H10 of O10, H13 of O13, H21 of O21, H7 of O7, All C(H,H)
  groups
 At 1.5 times of:
  H34 of O34, H25 of O25, H12 of O12, H38 of O38, H6AA of O6AA, H37 of O37,
  H4 of O4, H30A of O30, H3 of O3, H26A of O26, H20 of O20, H41A of O41, H17 of
  O17, H32 of O32
2. Restrained distances
 O37-H37
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 O30-H30A
 0.85 with sigma of 0.01
 O12-H12
 0.85 with sigma of 0.01
 O6AA-H6AA
 0.85 with sigma of 0.01
 O38-H38
 0.85 with sigma of 0.01
 O20-H20
 0.85 with sigma of 0.01
 O32-H32
 0.85 with sigma of 0.01
 O17-H17
 0.85 with sigma of 0.01
 O26-H26A
 0.85 with sigma of 0.01
 O3-H3
 0.85 with sigma of 0.01
 C48-H37
 1.880136 with sigma of 0.02
 Tb6-H37
 3.149753 with sigma of 0.02
 C6-H4
 1.874215 with sigma of 0.02
 Tb1-H4
 3.139343 with sigma of 0.02
 C87-H30A
 1.888347 with sigma of 0.02
 Tb4-H30A
 3.163259 with sigma of 0.02
 C36-H12
 1.888221 with sigma of 0.02
 Tb2-H12
 2.990153 with sigma of 0.02
 C74-H6AA
 1.903386 with sigma of 0.02
 Tb5-H6AA
 3.090232 with sigma of 0.02
 C46-H38
 1.895633 with sigma of 0.02
 Tb6-H38
 3.086148 with sigma of 0.02
 C23-H20
 1.889157 with sigma of 0.02
 Tb3-H20
 3.064817 with sigma of 0.02
 C89-H32
 1.893834 with sigma of 0.02
 Tb4-H32
 3.115626 with sigma of 0.02
 C21-H17
 1.89761 with sigma of 0.02
 Tb3-H17
 3.106099 with sigma of 0.02
 C72-H26A
 1.855448 with sigma of 0.02
 Tb5-H26A
 3.119408 with sigma of 0.02
 C8-H3
 1.87306 with sigma of 0.02
 Tb1-H3
 3.100557 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O25: within 2A with sigma of 0.0001 and sigma for terminal atoms of 0.002
Uanis(C38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 O13(H13), O21(H21), O7(H7), O10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C48(H48A,H48B), C74(H74A,H74B), C47(H47A,H47B), C34(H34A,
 H34B), C71(H71A,H71B), C87(H87A,H87B), C36(H36A,H36B), C73(H73A,H73B),
 C51(H51A,H51B), C70(H70A,H70B), C21(H21A,H21B), C52(H52A,H52B), C33(H33A,H33B),
  C89(H89A,H89B), C68(H68A,H68B), C37(H37A,H37B), C88(H88A,H88B), C49(H49A,
 H49B), C17(H17A,H17B), C23(H23A,H23B), C22(H22A,H22B), C86(H86A,H86B),
 C20(H20A,H20B), C46(H46A,H46B), C83(H83A,H83B), C85(H85A,H85B), C16(H16A,H16B),
  C50(H50A,H50B), C72(H72A,H72B), C19(H19A,H19B), C67(H67A,H67B), C1(H1A,H1B),
 C31(H31A,H31B), C6(H6A,H6B), C8(H8A,H8B), C82(H82A,H82B), C2(H2A,H2B), C7(H7A,
 H7B), C38(H38A,H38B), C5(H5A,H5B), C4(H4A,H4B)
4.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C26(H26), C60(H60), C57(H57), C62(H62), C61(H61), C15(H15),
 C81(H81), C59(H59), C58(H58), C14(H14), C64(H64), C42(H42), C63(H63), C44(H44),
  C28(H28), C77(H77), C45(H45), C43(H43), C11(H11), C55(H55), C41(H41),
 C27(H27), C29(H29), C12(H12A), C13(H13A), C78(H78), C79(H79), C80(H80),
 C56(H56)
4.d Tetrahedral OH refined with riding coordinates:
 O41(H41A), O34(H34)
4.e Idealised tetrahedral OH refined as rotating group:
 O25(H25)
;
_shelx_res_checksum              22363
_olex2_submission_special_instructions 'No special instructions were received'