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_7228693
_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 Gd6 N6 O42,2(H2O),C7 H8'
_chemical_formula_sum            'C97 H144 Gd6 N6 O44'
_chemical_formula_weight         3041.69
_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.cc1nv7qg
_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                   26.842(4)
_cell_length_b                   26.842(4)
_cell_length_c                   78.271(16)
_cell_measurement_reflns_used    27636
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.000
_cell_measurement_theta_min      1.019
_cell_volume                     48838(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_number            21319
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.019
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.7
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             27636
_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 for each hexanuclear ring.
;
_refine_diff_density_max         2.813
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.129
_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     1335
_refine_ls_number_reflns         21319
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      22.597
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+574.4930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20154
_reflns_number_total             21319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01063j2.cif
_cod_data_source_block           1
_cod_original_cell_volume        48838(17)
_cod_database_code               7228693
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H21 of O21, H30 of O30, All C(H,H) groups
 At 1.5 times of:
  H4 of O4, H3 of O3, H7 of O7, H38 of O38, H37 of O37, H41 of O41, H17 of
  O17, H10 of O10, H13 of O13, H12 of O12, H19 of O19, H26 of O26, H32A of O32,
  H5AA of O5AA, H25 of O25, H34A of O34
2. Restrained distances
 O32-H32
 0.85 with sigma of 0.01
 O30-H31
 0.85 with sigma of 0.01
 O3-H3
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 O12-H12
 0.85 with sigma of 0.01
 O13-H13
 0.85 with sigma of 0.01
 O17-H17
 0.85 with sigma of 0.01
 O19-H19
 0.85 with sigma of 0.01
 O5AA-H5AA
 0.85 with sigma of 0.01
 O26-H26
 0.85 with sigma of 0.01
 O37-H37
 0.85 with sigma of 0.01
 O38-H38
 0.85 with sigma of 0.01
 O32-H32A
 0.85 with sigma of 0.01
 C61-H32
 1.880457 with sigma of 0.02
 Gd4-H32
 3.016725 with sigma of 0.02
 C67-H31
 1.860227 with sigma of 0.02
 Gd4-H31
 3.092556 with sigma of 0.02
 C8-H3
 1.888437 with sigma of 0.02
 Gd1-H3
 3.16481 with sigma of 0.02
 C6-H4
 1.898391 with sigma of 0.02
 Gd1-H4
 3.084489 with sigma of 0.02
 C23-H12
 1.908177 with sigma of 0.02
 Gd2-H12
 3.097851 with sigma of 0.02
 C25-H13
 1.855828 with sigma of 0.02
 Gd2-H13
 3.128949 with sigma of 0.02
 C42-H17
 1.898065 with sigma of 0.02
 Gd3-H17
 3.127123 with sigma of 0.02
 C38-H19
 1.902389 with sigma of 0.02
 Gd3-H19
 3.193787 with sigma of 0.02
 C60-H5AA
 1.886212 with sigma of 0.02
 Gd5-H5AA
 3.082672 with sigma of 0.02
 C58-H26
 1.901985 with sigma of 0.02
 Gd5-H26
 3.124799 with sigma of 0.02
 C81-H37
 1.875206 with sigma of 0.02
 Gd6-H37
 3.119781 with sigma of 0.02
 C83-H38
 1.889961 with sigma of 0.02
 Gd6-H38
 3.145194 with sigma of 0.02
 C61-H32A
 1.8843 with sigma of 0.02
 Gd4-H32A
 3.014557 with sigma of 0.02
3.a Riding coordinates:
 O21(H21), O30(H30)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C38(H38A,H38B), C39(H39A,H39B),
  C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C45(H45A,
 H45B), C53(H53A,H53B), C54(H54A,H54B), C56(H56A,H56B), C57(H57A,H57B),
 C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B),
  C63(H63A,H63B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,
 H68B), C76(H76A,H76B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B),
 C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B)
3.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12A), C13(H13A), C14(H14), C15(H15), C16(H16), C17(H17A),
 C18(H18), C19(H19A), C20(H20), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C69(H69), C70(H70),
  C71(H71), C72(H72), C73(H73), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90)
3.d Idealised tetrahedral OH refined as rotating group:
 O7(H7), O10(H10), O25(H25), O34(H34A), O41(H41)
;
_shelx_res_checksum              32017
_olex2_submission_special_instructions 'No special instructions were received'