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_7044003
_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         '1(C39 H54 Eu1 N7 O3), 1.5(H2O)'
_chemical_formula_sum            'C39 H57 Eu N7 O4.5'
_chemical_formula_weight         847.88
_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
_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                   12.3525(17)
_cell_length_b                   12.3525(17)
_cell_length_c                   31.422(6)
_cell_measurement_reflns_used    2824
_cell_measurement_temperature    100
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2.6
_cell_volume                     4152.2(11)
_computing_cell_refinement       'ShelXL least squares'
_computing_data_collection       'Blue Ice'
_computing_data_reduction        XDS
_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      100.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.993
_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  0.0698
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_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       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            54585
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         1.904
_diffrn_source                   'MX1 Australian Synchrotron'
_exptl_absorpt_coefficient_mu    1.553
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1696
_exptl_crystal_preparation       'slow evaporation from MeOH and DCM mixture'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.039
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2831
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0407P)^2^+22.0586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2264
_reflns_number_total             2831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02556d2.cif
_cod_data_source_block           p-3c1_a
_cod_original_cell_volume        4152.2(16)
_cod_database_code               7044003
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
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)
;
_shelx_res_checksum              26199
_shelx_fab_checksum              48698
_olex2_submission_special_instructions 'No special instructions were received'