The Nature of the Bridging Anion Controls the Single-Molecule Magnetic Properties of DyX<sub>4</sub>M 12-Metallacrown-4 Complexes.
Boron, 3rd, Thaddeus T; Lutter, Jacob C.; Daly, Connor I.; Chow, Chun Y.; Davis, Andrew H.; Nimthong-Roldán, Arunpatcha; Zeller, Matthias; Kampf, Jeff W.; Zaleski, Curtis M.; Pecoraro, Vincent L.; Inorganic chemistry 55 (2016) 10597–10607; doi:10.1021/acs.inorgchem.6b01832

data_4348937
_publ_section_title
;
 The Nature of the Bridging Anion Controls the Single-Molecule Magnetic
 Properties of DyX<sub>4</sub>M 12-Metallacrown-4 Complexes.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10597
_journal_page_last               10607
_journal_paper_doi               10.1021/acs.inorgchem.6b01832
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C52.22 H67.04 Dy Mn4 N5.41 Na O24, 7(C3 H7 N O),0.592(H2 O)'
_chemical_formula_sum            'C73.22 H117.22 Dy Mn4 N12.41 Na O31.59'
_chemical_formula_weight         2082.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.528(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1240(12)
_cell_length_b                   18.9136(11)
_cell_length_c                   26.0448(17)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.6855
_cell_measurement_theta_min      2.6672
_cell_volume                     9290.5(10)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2014)'
_computing_data_collection       'Apex2 v2014.11 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker, 2014)'
_computing_structure_refinement
;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev714 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker AXS X8 Prospector CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            80387
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        66.790
_diffrn_reflns_theta_max         66.790
_diffrn_reflns_theta_min         2.667
_diffrn_source                   'I-mu-S microsource X-ray tube'
_exptl_absorpt_coefficient_mu    9.285
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2014.11 (Bruker, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       plate
_exptl_crystal_F_000             4292.6
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.698
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1447
_refine_ls_number_reflns         16256
_refine_ls_number_restraints     1687
_refine_ls_restrained_S_all      Infinity
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+40.6538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1569
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12105
_reflns_number_total             16256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01832_si_002.cif
_cod_data_source_block           Prosp15mz153_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4348937
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.258
_shelx_estimated_absorpt_t_max   0.654
_shelx_res_checksum              57181
_shelx_hkl_checksum              54432