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_4348936
_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 K Mn4 N4 O24, 4(C3 H7 N O), 1.6(H2 O)'
_chemical_formula_sum            'C68 H75.2 Dy K Mn4 N8 O29.6'
_chemical_formula_weight         1899.52
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 96.893(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1334(18)
_cell_length_b                   16.628(2)
_cell_length_c                   16.764(2)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.3042
_cell_measurement_theta_min      2.3518
_cell_volume                     3911.2(8)
_computing_cell_refinement       'SAINT V8.18C (Bruker, 2012)'
_computing_data_collection       'Apex2 v2012.4-3 (Bruker, 2012)'
_computing_data_reduction        'SAINT V8.18C (Bruker, 2012)'
_computing_molecular_graphics    'Shelxtl (Bruker, 2003)'
_computing_publication_material  'Shelxtl (Bruker, 2003)'
_computing_structure_refinement
;  
SHELXL-2013 (Sheldrick, 2013), 
SHELXLE Rev609 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44663
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.450
_diffrn_reflns_theta_min         2.163
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    1.712
_exptl_absorpt_correction_T_max  0.8640
_exptl_absorpt_correction_T_min  0.6428
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'Apex2 v2012.4-3 (Bruker, 2012)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       plate
_exptl_crystal_F_000             1922
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.353
_exptl_crystal_size_min          0.127
_refine_diff_density_max         2.136
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 10165 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.033(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1150
_refine_ls_number_reflns         22939
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+3.9740P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.835
_reflns_number_gt                22026
_reflns_number_total             22939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01832_si_002.cif
_cod_data_source_block           13mz129_0m
_cod_original_cell_volume        3911.2(9)
_cod_original_sg_symbol_H-M      'P n'
_cod_original_formula_sum        'C68 H75.20 Dy K Mn4 N8 O29.60'
_cod_database_code               4348936
_shelx_estimated_absorpt_t_min   0.525
_shelx_estimated_absorpt_t_max   0.812
_shelxl_version_number           2012-9
_shelx_res_checksum              78826
_shelx_hkl_checksum              90959