Slow magnetic dynamics in a family of mononuclear lanthanide complexes exhibiting the rare cubic coordination geometry.
Alexandropoulos, Dimitris I.; Schulte, Kelsey A.; Vignesh, Kuduva R.; Dunbar, Kim R.; Chemical communications (Cambridge, England) 54 (2018) 10136–10139; doi:10.1039/c8cc04565h

data_7122135
_publ_section_title
;
 Slow magnetic dynamics in a family of mononuclear lanthanide complexes
 exhibiting the rare cubic coordination geometry.
;
_journal_issue                   72
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10136
_journal_page_last               10139
_journal_paper_doi               10.1039/c8cc04565h
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C30 H22 N2 O10 Tb, 1.33(C18 H20 B2 Co1 N12)'
_chemical_formula_sum            'C54 H48.67 B2.67 Co1.33 N18 O10 Tb'
_chemical_formula_weight         1376.09
_space_group_crystal_system      cubic
_space_group_IT_number           197
_space_group_name_Hall           'I 2 2 3'
_space_group_name_H-M_alt        'I 2 3'
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-05 deposited with the CCDC.
2018-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   20.9135(4)
_cell_length_b                   20.9135(4)
_cell_length_c                   20.9135(4)
_cell_measurement_reflns_used    47411
_cell_measurement_temperature    100
_cell_measurement_theta_max      16.48
_cell_measurement_theta_min      2.27
_cell_volume                     9147.0(3)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3(Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008-2013)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 ' Pilatus1M(CdTe) pixel array detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS hybrid pixel array detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'huber three-circle diffractometer'
_diffrn_measurement_device_type  'Pilatus1M(CdTe) pixel array detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'Si 111 and Si 311'
_diffrn_radiation_probe          synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       2
_diffrn_reflns_number            3381
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         15.353
_diffrn_reflns_theta_min         1.387
_diffrn_source                   synchrotron
_diffrn_source_type              synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.6636
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1012 before and 0.0594 after correction. The Ratio of minimum to maximum transmission is 0.8919. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4158
_exptl_crystal_size_max          0.94
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.113
_platon_squeeze_details
;
TITL data_0m_b.res in I23
CELL   20.9135   20.9135   20.9135     90.00     90.00     90.00
SPGR I23
C101 0.138 0.010 0.008 !       1.57 eA-3
C102 0.012 0.855 0.047 !       1.21 eA-3
C103 0.436 0.507 0.336 !       1.17 eA-3
C104 0.922 0.868 0.987 !       1.14 eA-3
C105 0.422 0.368 0.487 !       1.14 eA-3
C106 0.093 0.120 1.003 !       1.10 eA-3
C107 0.481 0.545 0.422 !       0.73 eA-3
C108 0.484 0.515 0.485 !       0.72 eA-3
C109 0.940 0.049 0.090 !       0.58 eA-3
C110 0.491 0.491 0.491 !       0.55 eA-3
;
_refine_diff_density_max         0.403
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0277P)^2^+19.2636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3351
_reflns_number_total             3381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04565h2.cif
_cod_data_source_block           tb_dbm_no3_sq
_cod_depositor_comments
'Adding full bibliography for 7122134--7122137.cif.'
_cod_original_cell_volume        9147.0(5)
_cod_database_code               7122135
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.707
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(5)
 0.51(5)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
3.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C8(H8), C5(H5), C4(H4), C13(H13), C2(H2A), C10(H10),
 C7(H7), C6(H6), C9(H9), C14(H14)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'