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_4348935
_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
'C56 H44 Dy Mn4 N4 Na O24, 4(C3 H7 N O), H2 O'
_chemical_formula_sum            'C68 H66 Dy Mn4 N8 Na O29'
_chemical_formula_weight         1864.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 95.9290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.16570(10)
_cell_length_b                   16.57180(10)
_cell_length_c                   16.70750(10)
_cell_measurement_reflns_used    44773
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      72.8110
_cell_measurement_theta_min      2.6400
_cell_volume                     3901.12(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            87026
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.370
_diffrn_reflns_theta_min         2.666
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    10.951
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       block
_exptl_crystal_F_000             1878
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.690
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
; 
 Flack x determined using 6775 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.0125(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1214
_refine_ls_number_reflns         15186
_refine_ls_number_restraints     487
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+5.4182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.958
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                14627
_reflns_number_total             15186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01832_si_002.cif
_cod_data_source_block           tb2131
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4348935
_shelxl_version_number           2014/6
_shelx_res_checksum              70619
_shelx_hkl_checksum              52318