Crystallization of triple- and quadruple-stranded dinuclear bis-β-diketonate-Dy(iii) helicates: single molecule magnetic behavior
Chen, Peng; Li, Hongfeng; Sun, Wenbin; Tang, Jinkui; Zhang, Lei; Yan, Pengfei; CrystEngComm 17 (2015) 7227–; doi:10.1039/C5CE01067E

data_7221778
_publ_section_title
;
 Crystallization of triple- and quadruple-stranded dinuclear
 bis-\b-diketonate-Dy(iii) helicates: single molecule magnetic behavior
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              7227
_journal_paper_doi               10.1039/C5CE01067E
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C95 H72.5 Dy2 F18 N7.5 O14'
_chemical_formula_weight         2210.10
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-01 deposited with the CCDC.
2015-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                66.933(3)
_cell_angle_beta                 75.128(3)
_cell_angle_gamma                87.379(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1694(4)
_cell_length_b                   19.7909(5)
_cell_length_c                   21.6427(6)
_cell_measurement_reflns_used    14719
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.5620
_cell_measurement_theta_min      3.5260
_cell_volume                     4626.3(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            41308
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.706
_exptl_absorpt_correction_T_max  0.7838
_exptl_absorpt_correction_T_min  0.7486
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2202
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.573
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1251
_refine_ls_number_reflns         20844
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+5.0366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                17603
_reflns_number_total             20844
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01067e2.cif
_cod_data_source_block           1054123
_cod_depositor_comments
'Adding full bibliography for 7221777--7221779.cif.'
_cod_original_cell_volume        4626.3(2)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C95 H72.50 Dy2 F18 N7.50 O14'
_cod_database_code               7221778