A Series of CuII‒LnIII Metal‒Organic Frameworks Based on 2,2′-Bipyridine-3,3′-dicarboxylic Acid: Syntheses, Structures, and Magnetic Properties
Liu, Ke; Zhou, Jing-Min; Li, Hui-Min; Xu, Na; Cheng, Peng; Crystal Growth & Design 14 (2014) 6409–; doi:10.1021/cg5012617

data_4517093
_publ_section_title
;
 A Series of CuII--LnIII Metal--Organic Frameworks Based on
 2,2&#x2032;-Bipyridine-3,3&#x2032;-dicarboxylic Acid: Syntheses,
 Structures, and Magnetic Properties
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              6409
_journal_paper_doi               10.1021/cg5012617
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C48 H36 Cu3 Dy1 N9 O25'
_chemical_formula_sum            'C48 H36 Cu3 Dy N9 O25'
_chemical_formula_weight         1492.01
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-08-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                92.957(5)
_cell_angle_beta                 105.125(6)
_cell_angle_gamma                110.694(6)
_cell_formula_units_Z            2
_cell_length_a                   12.1832(9)
_cell_length_b                   14.8529(9)
_cell_length_c                   15.1970(9)
_cell_measurement_temperature    124.60(10)
_cell_measurement_theta_max      29.0222
_cell_measurement_theta_min      2.5408
_cell_volume                     2451.8(3)
_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      124.60(10)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega  -23.00   92.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.7135   19.0000 -150.0000 115

  2 omega   -4.00   61.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.7135  -99.0000  -30.0000 65

  3 omega    4.00   91.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       18.7135   37.0000   90.0000 87

  4 omega  -90.00  -34.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.2604  179.0000  150.0000 56

  5 omega  -33.00    1.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.2604  -84.0000   82.0000 34

  6 omega  -37.00   12.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.2604  -84.0000  158.0000 49

;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0312144000
_diffrn_orient_matrix_UB_12      0.0087082000
_diffrn_orient_matrix_UB_13      -0.0340063000
_diffrn_orient_matrix_UB_21      -0.0449928000
_diffrn_orient_matrix_UB_22      0.0156992000
_diffrn_orient_matrix_UB_23      -0.0266574000
_diffrn_orient_matrix_UB_31      0.0354199000
_diffrn_orient_matrix_UB_32      0.0484909000
_diffrn_orient_matrix_UB_33      0.0230513000
_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  0.0653
_diffrn_reflns_av_sigmaI/netI    0.1007
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16645
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    2.896
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.714
_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_colour            green
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         9.404
_refine_diff_density_min         -2.169
_refine_diff_density_rms         0.355
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         8472
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.1136
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+242.3737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2738
_refine_ls_wR_factor_ref         0.2825
_reflns_number_gt                7098
_reflns_number_total             8472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5012617_si_002.cif
_cod_data_source_block           10-DyCu3
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4517093
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_theta     26.32
_reflns_odcompleteness_iscentric 1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uains(C32) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uains(N2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uains(C7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uains(C19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uains(C26) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C45) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(N3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(O7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(O15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(N4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C31) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(N5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(N7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(O1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(O10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C25) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(O14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C18) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C40) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C22) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C27) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C46) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C16) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C21) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C31) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C48) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(O9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C33) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Rotating group:
 O9(H9a,H9b), O10(H10a,H10b),O11(H11a,H11b), O12(H12a,H12b), O22(H22a,H22b)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C27(H27), C28(H28), C29(H29), 
C32(H32), C33(H33), C34(H34), C39(H39), C40(H40), C41(H41), C44(H44), 
C45(H45), C46(H46)
;