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_7228691
_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 Dy6 N6 O42, 2(H2 O)'
_chemical_formula_sum            'C90 H136 Dy6 N6 O44'
_chemical_formula_weight         2981.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-01-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-07-14 deposited with the CCDC.
2017-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.76(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.664(7)
_cell_length_b                   11.254(2)
_cell_length_c                   30.378(6)
_cell_measurement_reflns_used    5784
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.279
_cell_measurement_theta_min      1.565
_cell_volume                     10371(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            13528
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        23.280
_diffrn_reflns_theta_max         23.279
_diffrn_reflns_theta_min         1.565
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.358
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_description       block
_exptl_crystal_F_000             5784
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.932
_refine_diff_density_min         -1.597
_refine_diff_density_rms         0.371
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         7436
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0942P)^2^+248.6464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6861
_reflns_number_total             7436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01063j2.cif
_cod_data_source_block           3
_cod_database_code               7228691
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C40-C41 = C41-C42 = C42-C43 = C43-C44 = C44-C45 = C45-C40
 1.45 with sigma of 0.01
 C40-C42 = C41-C43 = C42-C44 = C43-C45 = C44-C40 = C45-C41
 2.45 with sigma of 0.02
 O20-C39 = O21-C39
 1.25 with sigma of 0.01
 C39-C40
 1.45 with sigma of 0.01
 O20-C40 = O21-C40 = C39-C41 = C39-C45
 2.45 with sigma of 0.02
 O9-H9
 0.85 with sigma of 0.01
 O14-H14
 0.85 with sigma of 0.01
 O1-H1
 0.85 with sigma of 0.01
 O15-H15
 0.85 with sigma of 0.01
 O10-H10
 0.85 with sigma of 0.01
 O2-H2
 0.85 with sigma of 0.01
 C14-H9
 1.898829 with sigma of 0.02
 Dy2-H9
 3.00226 with sigma of 0.02
 C24-H14
 1.881453 with sigma of 0.02
 Dy3-H14
 3.003079 with sigma of 0.02
 C1-H1
 1.893546 with sigma of 0.02
 Dy1-H1
 3.057879 with sigma of 0.02
 C22-H15
 1.910557 with sigma of 0.02
 Dy3-H15
 3.119991 with sigma of 0.02
 C16-H10
 1.897896 with sigma of 0.02
 Dy2-H10
 3.121411 with sigma of 0.02
 C4-H2
 1.890814 with sigma of 0.02
 Dy1-H2
 3.066858 with sigma of 0.02
3. Restrained planarity
 C40, C41, C42, C43, C44, C45
 with sigma of 0.1
 O20, O21, C39, C40
 with sigma of 0.1
4. Rigid bond restraints
 O20, C39, O21, C40, C41, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O20 \\sim C39 \\sim O21 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim
C45: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B), C17(H17A,H17B), C7(H7A,H7B), C19(H19A,H19B),
 C6(H6A,H6B), C8(H8A,H8B), C10(H10A,H10B), C9(H9A,H9B), C21(H21A,H21B), C2(H2A,
 H2B), C1(H1A,H1B), C23(H23A,H23B), C22(H22A,H22B), C4(H4A,H4B), C3(H3A,H3B),
 C15(H15A,H15B), C24(H24A,H24B), C16(H16A,H16B), C13(H13A,H13B), C14(H14A,H14B)
6.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C27(H27), C36(H36), C37(H37), C35(H35), C28(H28), C29(H29),
 C34(H34), C31(H31), C30(H30), C43(H43), C42(H42), C44(H44), C41(H41), C45(H45)
6.c Idealised tetrahedral OH refined as rotating group:
 O8(H8), O13(H13), O5(H5)
;
_shelx_res_checksum              72226
_olex2_submission_special_instructions 'No special instructions were received'