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_7044002
_publ_section_title
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 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_absolute_configuration unk
_chemical_formula_moiety         'C39 H57 N7 O3'
_chemical_formula_sum            'C39 H57 N7 O3'
_chemical_formula_weight         671.93
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_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            6
_cell_length_a                   13.6115(19)
_cell_length_b                   13.6115(19)
_cell_length_c                   35.291(7)
_cell_measurement_reflns_used    33332
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.81
_cell_measurement_theta_min      2.88
_cell_volume                     5662.5(16)
_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      100.15
_diffrn_measured_fraction_theta_full 0.9857
_diffrn_measured_fraction_theta_max 0.8499
_diffrn_measurement_device_type  'ADSC Q315r CCD area-detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            33332
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         31.81
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'MX1 Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.076
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.1822
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2184.8532
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.5053
_refine_diff_density_min         -0.3478
_refine_diff_density_rms         0.0549
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.0(8)
_refine_ls_d_res_high            0.6741
_refine_ls_d_res_low             7.0635
_refine_ls_goodness_of_fit_ref   1.2796
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     153
_refine_ls_number_reflns         3668
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.2794
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.846
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              51
_reflns_limit_l_min              -51
_reflns_number_gt                3564
_reflns_number_total             3668
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt02556d2.cif
_cod_data_source_block           FL177_a
_cod_database_code               7044002
_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 C(H,H,H) groups
2. Restrained distances
 O1-H1
 0.87 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C10(H10a,H10b), C12(H12a,H12b)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C8(H8)
3.c Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C13(H13a,H13b,H13c)
;
_olex2_submission_special_instructions 'No special instructions were received'