Lanthanide coordination complexes framed by sodium ions: Slow relaxation of the magnetization in the Dy(ΙΙΙ) derivative.
Konstantatos, Andreas; Sørensen, Mikkel A.; Bendix, Jesper; Weihe, Høgni; Dalton Trans.  (2017) –; doi:10.1039/C7DT00863E

data_7042708
_publ_section_title
;
 Lanthanide coordination complexes framed by sodium ions: Slow relaxation
 of the magnetization in the Dy(\I\I\I) derivative.
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00863E
_journal_year                    2017
_chemical_formula_moiety
'C74 H84 Ho4 N10 Na2 O24, 4(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum            'C86 H116 Ho4 N14 Na2 O30'
_chemical_formula_weight         2531.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-09-27
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-03-09 deposited with the CCDC.
2017-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                63.278(5)
_cell_angle_beta                 77.736(5)
_cell_angle_gamma                63.411(5)
_cell_formula_units_Z            1
_cell_length_a                   13.847(2)
_cell_length_b                   14.479(2)
_cell_length_c                   14.893(2)
_cell_measurement_reflns_used    9566
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.08
_cell_measurement_theta_min      2.73
_cell_volume                     2384.7(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            119119
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    3.377
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0711 before and 0.0599 after correction.
The Ratio of minimum to maximum transmission is 0.9062.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.7627
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1260.5750
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.045
_refine_diff_density_max         2.0714
_refine_diff_density_min         -1.0154
_refine_diff_density_rms         0.1939
_refine_ls_d_res_high            0.7801
_refine_ls_d_res_low             7.4641
_refine_ls_goodness_of_fit_ref   1.0650
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    89
_refine_ls_number_parameters     634
_refine_ls_number_reflns         10526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0650
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+3.9091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              18
_reflns_limit_k_min              -16
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                8545
_reflns_number_total             10526
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt00863e2.cif
_cod_data_source_block           mo_D8V794_0m-new
_cod_original_cell_volume        2384.8(7)
_cod_database_code               7042708
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O15(H15a,H15b)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C12(H12), C20(H20), C24(H24), C26(H26),
 C27(H27), C31(H31), C34(H34), C35(H35), C37(H37), C39(H39), C42(H42), C45(H45),
  C47(H47), C49(H49), C50(H50), C25(H25), C41(H41)
2.c Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C9(H9a,H9b,H9c), C38(H38a,H38b,H38c),
 C40(H40a,H40b,H40c), C44(H44a,H44b,H44c), C46(H46a,H46b,H46c), C8(H8a,H8b,H8c),
  C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C48(H48a,H48b,H48c)
;
_olex2_submission_special_instructions 'No special instructions were received'