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_4348933
_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_absolute_configuration ad
_chemical_formula_moiety
;
 '(C58 H51.50 Dy K Mn4 N5.50 O28.50), 3.5(C3 H7 N O), 2(H2 O)0.5'
;
_chemical_formula_sum            'C68.5 H79 Dy K Mn4 N9 O33'
_chemical_formula_weight         1977.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90.90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.26430(10)
_cell_length_b                   24.32950(10)
_cell_length_c                   14.65880(10)
_cell_measurement_reflns_used    63800
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      72.9180
_cell_measurement_theta_min      2.6020
_cell_volume                     8295.99(8)
_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 0.995
_diffrn_measured_fraction_theta_max 0.982
_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  0.0384
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            92984
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.331
_diffrn_reflns_theta_min         3.633
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    10.767
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52720
_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    1.583
_exptl_crystal_description       prism
_exptl_crystal_F_000             4008
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
; 
 Flack x determined using 6699 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.0104(19)
_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     1153
_refine_ls_number_reflns         15415
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+9.4787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.883
_reflns_Friedel_fraction_full    0.897
_reflns_Friedel_fraction_max     0.869
_reflns_number_gt                14860
_reflns_number_total             15415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01832_si_002.cif
_cod_data_source_block           tb2138
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum        'C68.50 H79 Dy K Mn4 N9 O33'
_cod_database_code               4348933
_shelx_estimated_absorpt_t_min   0.295
_shelx_estimated_absorpt_t_max   0.412
_shelxl_version_number           2014/6
_shelx_res_checksum              43398
_shelx_hkl_checksum              65352