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_7044000
_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 Gd1 N7 O3), 1(C39 H51 Gd1 N7 O3), 4(H2O)'
_chemical_formula_sum            'C78 H113 Gd2 N14 O10'
_chemical_formula_weight         1721.3385
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_symmetry_space_group_name_Hall  'P 3 2"'
_symmetry_space_group_name_H-M   'P 3 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-08-17
_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            2
_cell_length_a                   12.3620(18)
_cell_length_b                   12.3620(18)
_cell_length_c                   31.321(6)
_cell_measurement_reflns_used    2884
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2.6
_cell_volume                     4145.2(12)
_computing_cell_refinement       Shelxl
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_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  0.0777
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.991
_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            56365
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         1.902
_diffrn_source                   'MX1 Australian Synchrotron'
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1694
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
TITL x_dummy   P 3 2 1      R = 0.08                                            
CELL   12.3620   12.3620   31.3210     90.00     90.00    120.00                
SPGR P321                                                                       
Q101 0.308 0.496 0.681 !       7.04 eA-3                                        
C102 0.261 0.645 0.204 !       6.30 eA-3                                        
C103 0.740 0.354 0.295 !       6.08 eA-3                                        
Q104 0.692 0.504 0.820 !       5.56 eA-3                                        
C105 0.671 0.347 0.333 !       5.39 eA-3                                        
C106 0.340 0.684 0.156 !       3.44 eA-3                                        
Q107 0.337 0.673 0.496 !       2.48 eA-3                                        
Q108 0.335 0.673 0.570 !       1.79 eA-3                                        
C109 0.284 0.769 0.693 !       1.10 eA-3                                        
Q110 0.391 0.797 0.016 !       1.00 eA-3                                        
C111 0.599 0.242 0.828 !       1.00 eA-3                                        
Q112 0.324 0.751 0.502 !       1.00 eA-3                                        
Q113 0.672 0.338 0.874 !       0.97 eA-3                                        
Q114 0.832 0.346 0.294 !       0.97 eA-3                                        
Q115 0.683 0.185 0.363 !       0.96 eA-3                                        
Q116 0.391 0.771 0.501 !       0.96 eA-3                                        
Q117 0.339 0.823 0.705 !       0.94 eA-3                                        
Q118 0.359 0.590 0.569 !       0.92 eA-3                                        
Q119 0.677 0.509 0.337 !       0.91 eA-3                                        
Q120 0.408 0.637 0.570 !       0.88 eA-3                                        
Q121 0.598 0.450 0.787 !       0.85 eA-3                                        
Q122 0.740 0.283 0.942 !       0.84 eA-3                                        
Q123 0.157 0.582 0.665 !       0.81 eA-3                                        
Q124 0.561 0.274 0.437 !       0.80 eA-3                                        
Q125 0.252 0.681 0.507 !       0.76 eA-3                                        
Q126 0.606 0.241 0.758 !       0.74 eA-3                                        
Q127 0.152 0.584 0.626 !       0.72 eA-3                                        
Q128 0.329 0.649 0.837 !       0.70 eA-3                                        
Q129 0.751 0.514 0.851 !       0.68 eA-3                                        
Q130 0.407 0.579 0.258 !       0.67 eA-3                                        
Q131 0.685 0.381 0.864 !       0.67 eA-3                                        
Q132 0.280 0.635 0.078 !       0.65 eA-3                                        
C133 0.253 0.683 0.233 !       0.64 eA-3                                        
Q134 0.543 0.812 0.172 !       0.63 eA-3                                        
Q135 0.371 0.735 0.047 !       0.63 eA-3                                        
Q136 0.138 0.464 0.712 !       0.62 eA-3                                        
Q137 0.800 0.353 0.952 !       0.61 eA-3                                        
Q138 0.190 0.523 0.221 !       0.60 eA-3                                        
Q139 0.612 0.338 0.007 !       0.60 eA-3                                        
Q140 0.429 0.189 0.307 !       0.60 eA-3                                        
Q141 0.513 0.316 0.282 !       0.57 eA-3                                        
Q142 0.861 0.011 0.701 !       0.57 eA-3                                        
Q143 0.719 0.719 0.500 !       0.57 eA-3                                        
Q144 0.340 0.663 0.766 !       0.57 eA-3                                        
Q145 0.655 0.385 0.008 !       0.56 eA-3                                        
Q146 0.641 0.095 0.312 !       0.55 eA-3                                        
Q147 0.339 0.541 0.539 !       0.55 eA-3                                        
Q148 0.377 0.189 0.289 !       0.55 eA-3                                        
Q149 0.828 0.490 0.697 !       0.53 eA-3                                        
Q150 0.925 0.716 0.592 !       0.53 eA-3                                        
Q151 0.763 0.379 0.859 !       0.52 eA-3                                        
Q152 0.595 0.776 0.156 !       0.52 eA-3                                        
Q153 0.907 0.415 0.319 !       0.51 eA-3                                        
Q154 0.328 0.657 0.325 !       0.51 eA-3                                        
Q155 0.544 0.746 0.741 !       0.51 eA-3                                        
;
_refine_diff_density_max         2.765
_refine_diff_density_min         -3.129
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Flack x determined using 1417 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         56365
_refine_ls_number_restraints     315
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0762
_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^)+(0.0782P)^2^+32.7586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1829
_refine_ls_wR_factor_ref         0.2115
_reflns_Friedel_coverage         0.737
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                34880
_reflns_number_total             56365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02556d2.cif
_cod_data_source_block           p-31c_c_sq
_cod_original_cell_volume        4145.2(15)
_cod_database_code               7044000
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1
 0
2. 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
3. Restrained distances
 N3A-C2 = N3A-C13A
 1.48 with sigma of 0.02
 C14A-C13A = C2-C1
 1.52 with sigma of 0.02
 C11A-C0AA \\sim C12A-C11A
 with sigma of 0.02
 C2-C1 \\sim C14A-C13A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C13A)
Uanis(C14A) = Uanis(C1)
Uanis(C5B) = Uanis(O1B)
5. 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
6. Others
 Fixed Sof: C1(0.6) H1A(0.6) H1B(0.6) H1C(0.6) C2(0.6) H2A(0.6) H2B(0.6)
 H11A(0.35) H11B(0.35) H11C(0.65) H11D(0.65) C12A(0.35) H12A(0.35) H12B(0.35)
 H12C(0.35) C13A(0.4) H13A(0.4) H13B(0.4) C14A(0.4) H14A(0.4) H14B(0.4)
 H14C(0.4) C0AA(0.65) H0AA(0.65) H0AB(0.65) H0AC(0.65)
 Fixed Uiso: H14A(0.07) H14B(0.07) H14C(0.07)
 Fixed X: H14A(1.04368) H14B(0.940949) H14C(0.95879)
 Fixed Y: H14A(0.63505) H14B(0.52063) H14C(0.65721)
 Fixed Z: H14A(0.20938) H14B(0.236909) H14C(0.24282)
7.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C2A(H2AA,H2AB), C2(H2A,H2B), C11A(H11A,H11B), C11A(H11C,H11D),
  C13A(H13A,H13B), C1B(H1BA,H1BB), C2B(H2BA,H2BB), C11B(H11E,H11F), C13B(H13C,
 H13D)
7.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C5A(H5A), C6A(H6A), C8A(H8A), C3B(H3B), C6B(H6B), C8B(H8B), C9B(H9B)
7.c X=CH2 refined with riding coordinates:
 C12B(H12D,H12E)
7.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C12A(H12A,H12B,H12C), C14B(H14D,H14E,H14F), C0AA(H0AA,H0AB,
 H0AC)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'