Structural diversity of luminescent lanthanide metal‒organic frameworks based on a V-shaped ligand
He, Yan-Fei; Chen, Di-Ming; Xu, Hang; Cheng, Peng; CrystEngComm 17 (2015) 2471–; doi:10.1039/C4CE02380C

data_7219173
_publ_section_title
;
 Structural diversity of luminescent lanthanide metal--organic frameworks
 based on a V-shaped ligand
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              2471
_journal_paper_doi               10.1039/C4CE02380C
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C45 H35 N O18 Tb2'
_chemical_formula_sum            'C45 H35 N O18 Tb2'
_chemical_formula_weight         1195.58
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2014-10-20 deposited with the CCDC.
2014-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.382(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3673(4)
_cell_length_b                   27.9636(9)
_cell_length_c                   16.8012(6)
_cell_measurement_reflns_used    10177
_cell_measurement_temperature    129.6(2)
_cell_measurement_theta_max      28.9260
_cell_measurement_theta_min      3.3510
_cell_volume                     4342.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      129.6(2)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   -3.00   35.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   57.0000  -90.0000 38

  2 omega  -43.00   37.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -57.0000  -30.0000 80

  3 omega  -84.00   -2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9747  -57.0000   90.0000 82

  4 omega  -14.00   11.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9747  -77.0000   60.0000 25

  5 omega  -87.00  -45.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9747  -77.0000   60.0000 42
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0003716000
_diffrn_orient_matrix_UB_12      0.0024062000
_diffrn_orient_matrix_UB_13      0.0419827000
_diffrn_orient_matrix_UB_21      -0.0766989000
_diffrn_orient_matrix_UB_22      0.0007736000
_diffrn_orient_matrix_UB_23      -0.0073342000
_diffrn_orient_matrix_UB_31      -0.0024747000
_diffrn_orient_matrix_UB_32      -0.0252432000
_diffrn_orient_matrix_UB_33      0.0038419000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19812
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.79
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.311
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.099
_refine_diff_density_min         -1.580
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         7568
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+26.1377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                6674
_reflns_number_total             7568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02380c2.cif
_cod_data_source_block           p140611d
_cod_depositor_comments
'Adding full bibliography for 7219168--7219173.cif.'
_cod_database_code               7219173
_chemical_oxdiff_formula         'C Tb'
_reflns_odcompleteness_completeness 99.80
_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 C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N1-C45 = N1-C44
 1.45 with sigma of 0.01
 N1-C44 \\sim N1-C45
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C45 \\sim N1 \\sim O16 \\sim C43 \\sim C44: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
5.a Riding coordinates:
 O18(H18a,H18b), O17(H17a,H17b)
5.b Me refined with riding coordinates:
 C45(H45a,H45b,H45c), C44(H44a,H44b,H44c)
5.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C26(H26), C27(H27), C20(H20), C21(H21), C17(H17),
 C18(H18), C4(H4), C3(H3), C7(H7), C6(H6), C13(H13), C12(H12), C10(H10), C9(H9),
  C37(H37), C38(H38), C40(H40), C41(H41), C34(H34), C35(H35), C31(H31),
 C32(H32), C43(H43)
;
_olex2_submission_special_instructions 'No special instructions were received'