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_7219169
_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         '0.25(C200 H184 N8 O76 Tb8)'
_chemical_formula_sum            'C50 H46 N2 O19 Tb2'
_chemical_formula_weight         1296.73
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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_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                 107.423(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.379(2)
_cell_length_b                   8.9963(4)
_cell_length_c                   20.1175(14)
_cell_measurement_reflns_used    6159
_cell_measurement_temperature    130.4(2)
_cell_measurement_theta_max      28.8960
_cell_measurement_theta_min      3.4600
_cell_volume                     5245.8(6)
_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      130.4(2)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -20.00    6.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -99.0000  -90.0000 26

  2 omega  -40.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9747   37.0000  -30.0000 93

  3 omega  -37.00  -11.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9747   57.0000   60.0000 26

  4 omega    5.00   49.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9747   57.0000   60.0000 44

  5 omega  -87.00  -45.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9747 -178.0000   30.0000 42

  6 omega  -96.00  -50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9747  178.0000  120.0000 46
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0058946000
_diffrn_orient_matrix_UB_12      -0.0432903000
_diffrn_orient_matrix_UB_13      0.0308763000
_diffrn_orient_matrix_UB_21      -0.0151455000
_diffrn_orient_matrix_UB_22      0.0431760000
_diffrn_orient_matrix_UB_23      0.0130051000
_diffrn_orient_matrix_UB_31      -0.0182816000
_diffrn_orient_matrix_UB_32      -0.0497922000
_diffrn_orient_matrix_UB_33      -0.0156051000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11976
_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    2.750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78803
_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    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         11.209
_refine_diff_density_min         -1.739
_refine_diff_density_rms         0.384
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4615
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0794
_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^)+(0.1522P)^2^+107.5470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2169
_reflns_number_gt                4118
_reflns_number_total             4615
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02380c2.cif
_cod_data_source_block           p140427j
_cod_depositor_comments
'Adding full bibliography for 7219168--7219173.cif.'
_cod_original_cell_volume        5245.9(6)
_cod_database_code               7219169
_chemical_oxdiff_formula         'C Tb'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C25-N1A \\sim N1A-C24B
 with sigma of 0.02
 C23A-N1B \\sim N1B-C25
 with sigma of 0.02
 C23B-C22A \\sim C22B-C24A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O9 \\sim N1B \\sim C25 \\sim C22B: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C11A) \\sim Ueq, Uanis(O8A) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C12A)
\\sim Ueq, Uanis(C11B) \\sim Ueq, Uanis(C12B) \\sim Ueq, Uanis(C13B) \\sim Ueq,
Uanis(O8B) \\sim Ueq, Uanis(C16B) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C16A)
\\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C19A) \\sim Ueq,
Uanis(C18A) \\sim Ueq, Uanis(C21B) \\sim Ueq, Uanis(C20B) \\sim Ueq,
Uanis(C19B) \\sim Ueq, Uanis(C18B) \\sim Ueq, Uanis(C17B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
Uanis(C24A) \\sim Ueq, Uanis(C24B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C23B) \\sim Ueq, Uanis(C23A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C11A) = Uanis(C11B)
Uanis(C12A) = Uanis(C12B)
Uanis(C13A) = Uanis(C13B)
Uanis(O8A) = Uanis(O8B)
Uanis(C16A) = Uanis(C16B)
Uanis(C21A) = Uanis(C21B)
Uanis(C20A) = Uanis(C20B)
Uanis(C19A) = Uanis(C19B)
Uanis(C18A) = Uanis(C18B)
Uanis(C17A) = Uanis(C17B)
Uanis(C22B) = Uanis(C22A)
Uanis(N1A) = Uanis(N1B)
Uanis(C23A) = Uanis(C23B)
Uanis(C24A) = Uanis(C24B)
4. Others
 Sof(H14a)=Sof(C11A)=Sof(H11A)=Sof(O8A)=Sof(C13A)=Sof(C12A)=Sof(H12A)=1-FVAR(1)
 Sof(H14)=Sof(C11B)=Sof(H11B)=Sof(C12B)=Sof(H12B)=Sof(C13B)=Sof(O8B)=FVAR(1)
 Sof(C17A)=Sof(H17A)=Sof(C16A)=Sof(C21A)=Sof(H21A)=Sof(C20A)=Sof(H20A)=
 Sof(C19A)=Sof(C18A)=Sof(H18A)=1-FVAR(2)
 Sof(C16B)=Sof(C21B)=Sof(H21B)=Sof(C20B)=Sof(H20B)=Sof(C19B)=Sof(C18B)=
 Sof(H18B)=Sof(C17B)=Sof(H17B)=FVAR(2)
 Sof(N1B)=Sof(H25d)=Sof(H25e)=Sof(H25f)=Sof(C24A)=Sof(H24a)=Sof(H24b)=
 Sof(H24c)=Sof(C23A)=Sof(H23a)=Sof(H23b)=Sof(H23c)=Sof(C22B)=1-FVAR(3)
 Sof(H25a)=Sof(H25b)=Sof(H25c)=Sof(N1A)=Sof(C22A)=Sof(C23B)=Sof(H23d)=
 Sof(H23e)=Sof(H23f)=Sof(C24B)=Sof(H24d)=Sof(H24e)=Sof(H24f)=FVAR(3)
5.a Rotating group:
 O10(H10a,H10b)
5.b Me refined with riding coordinates:
 C25(H25d,H25e,H25f), C25(H25a,H25b,H25c)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C15(H15), C2(H2), C6(H6), C14(H14a), C14(H14), C11A(H11A),
 C17A(H17A), C21A(H21A), C20A(H20A), C18A(H18A), C12A(H12A), C11B(H11B),
 C12B(H12B), C21B(H21B), C20B(H20B), C18B(H18B), C17B(H17B)
5.d Fitted hexagon refined as free rotating group:
 C17A(C16A,C21A,C20A,C19A,C18A), C16B(C21B,C20B,C19B,C18B,C17B)
5.e Idealised Me refined as rotating group:
 C24A(H24a,H24b,H24c), C23A(H23a,H23b,H23c), C23B(H23d,H23e,H23f), C24B(H24d,
 H24e,H24f)
;
_olex2_submission_special_instructions 'No special instructions were received'