Neutral dicyanidoferrate(II) metalloligands for the rational design of dysprosium(III) single-molecule magnets
Liberka, Michal; Zychowicz, Mikolaj; Zychowicz, Wiktor; Chorazy, Szymon; Chemical Communications  (2022) –; doi:10.1039/D2CC02238A

data_7130056
_publ_section_title
;
 Neutral dicyanidoferrate(II) metalloligands for the rational design of
 dysprosium(III) single-molecule magnets
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02238A
_journal_year                    2022
_chemical_formula_moiety
'C128 H100 Dy2 Fe4 N28 O8, 6[CF3O3S], 5[CH4O]'
_chemical_formula_sum            'C139 H120 Dy2 F18 Fe4 N28 O31 S6'
_chemical_formula_weight         3761.37
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      56
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   mixed
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_creation_date             2022-04-28T11:59:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2022-04-30 deposited with the CCDC.	2022-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.6454(9)
_cell_length_b                   25.4847(11)
_cell_length_c                   14.6915(5)
_cell_measurement_reflns_used    45070
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.027
_cell_measurement_theta_min      2.539
_cell_measurement_wavelength     0.71073
_cell_volume                     7729.8(5)
_computing_cell_refinement       'SAINT (Bruker, 2021)'
_computing_data_collection       'APEX4 (Bruker, 2021)'
_computing_data_reduction        'SAINT (Bruker, 2021)'
_computing_molecular_graphics    'Mercury 2021.1.0 (Macrae, 2020)'
_computing_publication_material
'WinGX publication routines (Farrugia, 2012), Olex2 (Dolomonov, 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'D8Quest Eco Photon50'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45070
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.539
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.503
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2728
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.52
_refine_diff_density_min         -4.254
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6822
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+65.0261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1596
_reflns_Friedel_coverage         0
_reflns_number_gt                5560
_reflns_number_total             6822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02238a2.cif
_cod_data_source_block           compound_4
_cod_database_code               7130056
_shelx_shelxl_version_number     2018/3
_smtbx_masks_special_details
;
A solvent mask was calculated and 1052 electrons were 
found in a volume of 2840\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 6[CF3O3S] and 
5[CH4O] per Formula Unit which account for 1056 electrons
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              55271
_shelx_hkl_checksum              50551