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_7221779
_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            'C17 H17 N O2'
_chemical_formula_weight         267.32
_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                94.615(7)
_cell_angle_beta                 98.690(7)
_cell_angle_gamma                99.967(7)
_cell_formula_units_Z            2
_cell_length_a                   8.2376(6)
_cell_length_b                   8.5362(7)
_cell_length_c                   10.4219(9)
_cell_measurement_reflns_used    5518
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.66
_cell_measurement_theta_min      3.30
_cell_volume                     709.21(10)
_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 0.994
_diffrn_measured_fraction_theta_max 0.847
_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  0.0143
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5518
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.774
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.129
_refine_diff_density_rms         0.030
_refine_ls_extinction_coef       0.032(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.0785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                2182
_reflns_number_total             3204
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01067e2.cif
_cod_data_source_block           1054124
_cod_depositor_comments
'Adding full bibliography for 7221777--7221779.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7221779