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_7122137
_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_absolute_configuration ad
_chemical_formula_moiety         'C30 H22 Er N2 O10, 1.33(C18 H20 B2 Co1 N12)'
_chemical_formula_sum            'C54 H48.67 B2.67 Co1.33 Er N18 O10'
_chemical_formula_weight         1384.43
_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                   20.9076(4)
_cell_length_b                   20.9076(4)
_cell_length_c                   20.9076(4)
_cell_measurement_reflns_used    91606
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.60
_cell_measurement_theta_min      2.27
_cell_volume                     9139.3(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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_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 0.998
_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  0.0431
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       2
_diffrn_reflns_number            7435
_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         20.178
_diffrn_reflns_theta_min         1.387
_diffrn_source                   synchrotron
_diffrn_source_type              synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1557 before and 0.0577 after correction. The Ratio of minimum to maximum transmission is 0.9267. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.214
_platon_squeeze_details
;
TITL data_0m_a.res in I23
CELL   20.9076   20.9076   20.9076     90.00     90.00     90.00
SPGR I23
C101 0.509 0.658 0.428 !       1.41 eA-3
C102 0.136 1.000 0.000 !       1.39 eA-3
Q103 0.516 1.000 0.000 !       1.12 eA-3
C104 0.955 0.017 0.134 !       1.12 eA-3
C105 0.657 0.508 0.440 !       1.00 eA-3
C106 0.063 0.153 0.993 !       1.00 eA-3
C107 0.862 0.008 0.088 !       0.96 eA-3
C108 0.507 0.619 0.336 !       0.94 eA-3
C109 0.837 0.030 0.018 !       0.90 eA-3
C110 0.820 0.017 0.038 !       0.80 eA-3
C111 0.883 0.122-0.001 !       0.78 eA-3
C112 0.960 0.826 0.057 !       0.63 eA-3
C113 0.095 0.014 0.051 !       0.61 eA-3
Q114 0.398 0.330 0.434 !       0.61 eA-3
Q115 0.602 0.326 0.559 !       0.61 eA-3
Q116 0.958 0.197 0.083 !       0.60 eA-3
Q117 0.572 0.565 0.298 !       0.57 eA-3
Q118 0.192 0.048 0.078 !       0.57 eA-3
C119 0.655 0.481 0.436 !       0.56 eA-3
C120 0.536 0.363 0.384 !       0.52 eA-3
C121 0.986 0.014 0.014 !       0.51 eA-3
;
_refine_diff_density_max         1.702
_refine_diff_density_min         -3.760
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         7435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+13.3852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1208
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7091
_reflns_number_total             7435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04565h2.cif
_cod_data_source_block           er_dbm_no3_sq
_cod_depositor_comments
'Adding full bibliography for 7122134--7122137.cif.'
_cod_original_cell_volume        9139.3(5)
_cod_database_code               7122137
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.897
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(3)
 0.45(3)
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:
 C9(H9), C10(H10), C2(H2A), C12(H12), C5(H5), C4(H4), C6(H6), C11(H11), C7(H7),
  C13(H13), C8(H8), C14(H14)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'