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_7219170
_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 Eu O12, 3(C3 H7 N O)'
_chemical_formula_sum            'C37 H41 Eu N3 O15'
_chemical_formula_weight         919.69
_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     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                85.350(4)
_cell_angle_beta                 76.570(4)
_cell_angle_gamma                72.158(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4805(4)
_cell_length_b                   13.8989(7)
_cell_length_c                   16.6460(9)
_cell_measurement_reflns_used    8304
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7360
_cell_measurement_theta_min      3.5420
_cell_volume                     2030.71(18)
_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      293(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   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -99.0000  -60.0000 26

  2 omega  -12.00   86.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   77.0000    0.0000 98

  3 omega  -10.00   84.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   77.0000 -150.0000 94

  4 omega  -48.00   45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -77.0000   90.0000 93

  5 omega  -76.00    3.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185  -19.0000 -120.0000 79
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0782692000
_diffrn_orient_matrix_UB_12      0.0086708000
_diffrn_orient_matrix_UB_13      0.0180921000
_diffrn_orient_matrix_UB_21      -0.0032726000
_diffrn_orient_matrix_UB_22      -0.0362891000
_diffrn_orient_matrix_UB_23      -0.0265671000
_diffrn_orient_matrix_UB_31      0.0187295000
_diffrn_orient_matrix_UB_32      -0.0385034000
_diffrn_orient_matrix_UB_33      0.0297677000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14085
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.615
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65085
_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    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         7148
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0311P)^2^+1.4680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                6409
_reflns_number_total             7148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02380c2.cif
_cod_data_source_block           p140604f
_cod_depositor_comments
'Adding full bibliography for 7219168--7219173.cif.'
_cod_original_cell_volume        2030.70(18)
_cod_database_code               7219170
_chemical_oxdiff_formula         C1H1O1N1EU1
_chemical_oxdiff_usercomment     5-21-6
_reflns_odcompleteness_completeness 99.84
_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. Restrained distances
 C1A-N2 = N2-C1B
 1.45 with sigma of 0.02
 H1Bc-H1Ac
 2.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O15 \\sim C13 \\sim N2 \\sim C1B \\sim C1A: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C1B) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
4.a Rotating group:
 O11(H11a,H11b), O12(H12a)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C15(H15), C17(H17), C18(H18),
 C20(H20), C21(H21), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C33(H33),
  C73(H73), C83(H83), C13(H13)
4.c Idealised Me refined as rotating group:
 C75(H75a,H75b,H75c), C76(H76a,H76b,H76c), C85(H85a,H85b,H85c), C86(H86a,H86b,
 H86c), C1A(H1Aa,H1Ab,H1Ac), C1B(H1Ba,H1Bb,H1Bc)
4.d Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'