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_4517092
_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         'C60 H42 Cu2 N10 O35 Tb2'
_chemical_formula_sum            'C60 H42 Cu2 N10 O35 Tb2'
_chemical_formula_weight         1908.00
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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                90.00
_cell_angle_beta                 98.299(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2520(10)
_cell_length_b                   22.3034(9)
_cell_length_c                   27.1573(15)
_cell_measurement_temperature    125.1(2)
_cell_measurement_theta_max      28.9640
_cell_measurement_theta_min      2.4183
_cell_volume                     6744.0(8)
_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      125.1(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -15.00   11.25   0.7500   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5573   89.0000   24.0000 35

  2 omega  -37.00   49.25   0.7500   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5573    0.0000  -30.0000 115
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0117122000
_diffrn_orient_matrix_UB_12      -0.0062154000
_diffrn_orient_matrix_UB_13      -0.0332876000
_diffrn_orient_matrix_UB_21      -0.0079184000
_diffrn_orient_matrix_UB_22      0.0134439000
_diffrn_orient_matrix_UB_23      0.0044288000
_diffrn_orient_matrix_UB_31      0.0066947000
_diffrn_orient_matrix_UB_32      0.0050203000
_diffrn_orient_matrix_UB_33      -0.0530513000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24429
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.45
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.800
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_correction_T_min  0.577
_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    1.879
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flaky
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.870
_refine_diff_density_min         -2.507
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         11891
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0711
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0844P)^2^+96.9116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.1914
_reflns_number_gt                9707
_reflns_number_total             11891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5012617_si_002.cif
_cod_data_source_block           9-Tb2Cu2
_cod_original_sg_symbol_Hall     '-p 2ybc'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4517092
_reflns_odcompleteness_completeness 99.8
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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(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(O4) \\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(O15) \\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
Uains(C50) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(N11) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uains(O21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uains(C62) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 
0.0002
Uains(C61) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 
0.0002
Uains(C60) \\sim Ueq: with sigma of 0.0005 and sigma for terminal atoms of 
0.001
Uains(O20) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C63) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(O19) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C56) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C57) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C58) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C59) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(N10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C55) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C41) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C6) \\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(C1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C19) \\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(C20) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C13) \\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(C34) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C35) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C24) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C43) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C42) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uains(C21) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 
0.0002
Uains(C51) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 
0.0002
3.a Rotating group:
 O21(H21a,H21b), O22(H22a,H22b),O23(H23a,H23b), O24(H24a,H24b), O25(H25a,H25b), 
O26(H26a,H26b)
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), C47(H47), C51(H51), C52(H52), C53(H53), C57(H57), C58(H58), 
C59(H59), C60(H60), C61(H61),C62(H62)
;