Synthesis and Characterisation of New Tripodal Lanthanide Complexes and Investigation of Their Optical and Magnetic Properties
Craze, Alexander R.; Huang, Xin-Da; Etchells, Isaac; Zheng, Li-Min; Bhadbhade, Mohan; Marjo, Christopher; Clegg, Jack Kay; Moore, Evan G.; Avdeev, Maxim; Lindoy, Leonard F.; Li, Feng; Dalton Trans.  (2017) –; doi:10.1039/C7DT02556D

data_7044001
_publ_section_title
;
 Synthesis and Characterisation of New Tripodal Lanthanide Complexes and
 Investigation of Their Optical and Magnetic Properties
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02556D
_journal_year                    2017
_chemical_formula_moiety         'C39 H54 Dy1 N7 O3, 3(H2 O)'
_chemical_formula_sum            'C39 H60 Dy N7 O6'
_chemical_formula_weight         885.4463
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2017-08-18 deposited with the CCDC.
2017-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   12.3876(10)
_cell_length_b                   12.3876(10)
_cell_length_c                   31.693(3)
_cell_measurement_reflns_used    9805
_cell_measurement_temperature    150.02
_cell_measurement_theta_max      27.189
_cell_measurement_theta_min      1.285
_cell_volume                     4211.8(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Apex II (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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.892
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            50279
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.189
_diffrn_reflns_theta_min         1.285
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.816
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1637 before and 0.0806 after correction.
The Ratio of minimum to maximum transmission is 0.8142.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1708
_exptl_crystal_preparation       'Slow evaporation from a MeOH/DCM mixture'
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.328
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2861
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.331
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0729P)^2^+3.6176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2149
_reflns_number_total             2861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02556d2.cif
_cod_data_source_block           sandy_dy_01sept16_2nd_0ma
_cod_original_cell_volume        4211.9(8)
_cod_database_code               7044001
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13'-C12A = C11'-C10 = C11-C10
 1.5 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C11'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H10C(0.3) H10D(0.3) H10A(0.7) H10B(0.7) C11'(0.3) H11C(0.3)
 H11B(0.3) H11A(0.3) C11(0.7) H11D(0.7) H11E(0.7) H11F(0.7) C13'(0.2) H13A(0.2)
 H13B(0.2) H13C(0.2) C13(0.8) H13D(0.8) H13E(0.8) H13F(0.8) H12D(0.2) H12C(0.2)
 H12A(0.8) H12B(0.8)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10C,H10D), C10(H10A,H10B), C12A(H12D,H12C),
 C12A(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C8(H8)
5.c Idealised Me refined as rotating group:
 C11'(H11C,H11B,H11A), C11(H11D,H11E,H11F), C13'(H13A,H13B,H13C), C13(H13D,
 H13E,H13F)
;
_shelx_res_checksum              76801
_shelx_fab_checksum              59280
_olex2_submission_special_instructions 'No special instructions were received'