Slow magnetic relaxation in four square-based pyramidal dysprosium hydroxo clusters ligated by chiral amino acid anions - a comparative study.
Thielemann, Dominique T.; Wagner, Anna T.; Lan, Yanhua; Anson, Christopher E.; Gamer, Michael T.; Powell, Annie K.; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 14794–14800; doi:10.1039/c3dt50133g

data_7021868
_publ_section_title
;
 Slow magnetic relaxation in four square-based pyramidal dysprosium
 hydroxo clusters ligated by chiral amino acid anions - a comparative
 study.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14794
_journal_page_last               14800
_journal_paper_doi               10.1039/c3dt50133g
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C122 H103 Dy5 N4 O25, 3(C H2 Cl2)'
_chemical_formula_sum            'C125 H109 Cl6 Dy5 N4 O25'
_chemical_formula_weight         3092.36
_chemical_name_systematic
;
?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2305(5)
_cell_length_b                   18.9609(4)
_cell_length_c                   33.7647(6)
_cell_measurement_reflns_used    55860
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      1.55
_cell_volume                     11671.3(5)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H.
Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H.
Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            51121
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_min         1.550
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.375
_exptl_absorpt_correction_T_max  0.6540
_exptl_absorpt_correction_T_min  0.2628
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       prism
_exptl_crystal_F_000             6076
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.280
_platon_squeeze_details
;
Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
Flack x determined using 7763 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.034(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1408
_refine_ls_number_reflns         21132
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0253P)^2^]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0619
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                18429
_reflns_number_total             21132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt50133g.txt
_cod_data_source_block           1
_cod_database_code               7021868
_shelx_estimated_absorpt_t_min   0.312
_shelx_estimated_absorpt_t_max   0.452