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_7219171
_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         'C28 H21 O12 Tb, 3(C3 H7 N O)'
_chemical_formula_sum            'C37 H42 N3 O15 Tb'
_chemical_formula_weight         927.66
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                85.363(4)
_cell_angle_beta                 76.965(5)
_cell_angle_gamma                72.239(5)
_cell_formula_units_Z            2
_cell_length_a                   9.3955(5)
_cell_length_b                   13.8663(6)
_cell_length_c                   16.5559(10)
_cell_measurement_reflns_used    9517
_cell_measurement_temperature    130.30(14)
_cell_measurement_theta_max      28.6390
_cell_measurement_theta_min      3.1420
_cell_volume                     2001.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      130.30(14)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -50.00   43.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -37.0000  -60.0000 93

  2 omega  -17.00   59.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -99.0000 -150.0000 76

  3 omega  -12.00   83.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   77.0000   90.0000 95

  4 omega   46.00   72.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372 -178.0000   90.0000 26

  5 omega  -88.00  -54.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185  -57.0000   30.0000 34

  6 omega  -84.00   11.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185  -77.0000  -90.0000 95
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0032751000
_diffrn_orient_matrix_UB_12      0.0499273000
_diffrn_orient_matrix_UB_13      -0.0109033000
_diffrn_orient_matrix_UB_21      0.0027230000
_diffrn_orient_matrix_UB_22      0.0079098000
_diffrn_orient_matrix_UB_23      0.0413505000
_diffrn_orient_matrix_UB_31      0.0809969000
_diffrn_orient_matrix_UB_32      -0.0181729000
_diffrn_orient_matrix_UB_33      -0.0102695000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14824
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         7050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.3005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0726
_reflns_number_gt                6477
_reflns_number_total             7050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02380c2.cif
_cod_data_source_block           p140616b
_cod_depositor_comments
'Adding full bibliography for 7219168--7219173.cif.'
_cod_original_cell_volume        2001.02(19)
_cod_database_code               7219171
_chemical_oxdiff_formula         C1H1O1N1TB1
_chemical_oxdiff_usercomment     5-27-2
_reflns_odcompleteness_completeness 99.85
_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) groups, All O(H,H) groups
2.a Rotating group:
 O40(H40a), O41(H41a,H41b)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C20(H20), C9(H9), C26(H26), C27(H27), C18(H18), C23(H23), C21(H21),
 C10(H10), C13(H13), C24(H24), C37(H37), C7(H7), C31(H31), C6(H6), C12(H12),
 C3(H3), C34(H34), C4(H4)
2.c Idealised Me refined as rotating group:
 C33(H33a,H33b,H33c), C35(H35a,H35b,H35c), C36(H36a,H36b,H36c), C29(H29a,H29b,
 H29c), C32(H32a,H32b,H32c), C30(H30a,H30b,H30c)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'