Constraining and Tuning the Coordination Geometry of a Lanthanide Ion in Metal-Organic Frameworks: Approach toward a Single-Molecule Magnet.
Liu, Ke; Li, Huanhuan; Zhang, Xuejing; Shi, Wei; Cheng, Peng; Inorganic chemistry 54 (2015) 10224–10231; doi:10.1021/acs.inorgchem.5b01356

data_1540019
_publ_section_title
;
 Constraining and Tuning the Coordination Geometry of a Lanthanide Ion in
 Metal-Organic Frameworks: Approach toward a Single-Molecule Magnet.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10224
_journal_page_last               10231
_journal_paper_doi               10.1021/acs.inorgchem.5b01356
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C26 H28 Dy2 N2 O19'
_chemical_formula_sum            'C26 H28 Dy2 N2 O19'
_chemical_formula_weight         997.50
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.465(5)
_cell_length_b                   9.2442(14)
_cell_length_c                   19.699(5)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9324
_cell_measurement_theta_min      2.4286
_cell_volume                     3286.8(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5599
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    4.597
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_correction_T_min  0.415
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flaky
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.029
_refine_diff_density_min         -2.687
_refine_diff_density_rms         0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2893
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0705
_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^)+(0.0918P)^2^+63.3123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1792
_refine_ls_wR_factor_ref         0.1965
_reflns_number_gt                2048
_reflns_number_total             2893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01356_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 1540018--1540020.cif.'
_cod_original_cell_volume        3286.7(13)
_cod_database_code               1540019
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
 C11 \\sim N1: within 1.7A with sigma of 0.001 and sigma for
terminal atoms of 0.002
 N1 \\sim C10: within 1.7A with sigma of 0.001 and sigma for
terminal atoms of 0.002
 CC \\sim C3: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Rotating group:
C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C4(H4A,H4B,H4C),O3(H3)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C7(H7), C10(H10)
;