Two series of pH-dependent lanthanide complexes showing solvent-induced single crystal to single crystal transformation, sorption and luminescence properties
Zhang, Lina; Zhang, Chao; Zhang, Bin; Du, Chenxia; Hou, Hongwei; CrystEngComm 17 (2015) 2837–; doi:10.1039/C5CE00263J

data_7219694
_publ_section_title
;
 Two series of pH-dependent lanthanide complexes showing solvent-induced
 single crystal to single crystal transformation, sorption and
 luminescence properties
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2837
_journal_paper_doi               10.1039/C5CE00263J
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety
'C73.5 H53 N1.5 O22 Tb2, C3 H6 N O, C3 H7 N O'
_chemical_formula_sum            'C79.5 H71.5 N3.5 O24 Tb2'
_chemical_formula_weight         1777.19
_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             2014-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2012.05.09 svn.r2324, GUI svn.r4862)
;
_audit_update_record
;
2015-01-16 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.034(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0878(3)
_cell_length_b                   29.4702(7)
_cell_length_c                   18.4237(4)
_cell_measurement_reflns_used    10302
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      29.2273
_cell_measurement_theta_min      2.8986
_cell_volume                     7313.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -24.00    5.00   1.0000   54.8200
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000   30.0000 29

  2 omega  -13.00   25.00   1.0000   54.8200
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000 -150.0000 38

  3 omega   32.00   80.00   1.0000   54.8200
omega____ theta____ kappa____ phi______ frames
    -       19.7104 -178.0000   90.0000 48

  4 omega  -38.00   79.00   1.0000   54.8200
omega____ theta____ kappa____ phi______ frames
    -       19.7104    0.0000    0.0000 117
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0320665000
_diffrn_orient_matrix_UB_12      -0.0173461000
_diffrn_orient_matrix_UB_13      -0.0199735000
_diffrn_orient_matrix_UB_21      -0.0411708000
_diffrn_orient_matrix_UB_22      0.0148196000
_diffrn_orient_matrix_UB_23      -0.0054474000
_diffrn_orient_matrix_UB_31      0.0070450000
_diffrn_orient_matrix_UB_32      0.0076850000
_diffrn_orient_matrix_UB_33      -0.0345276000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31944
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    2.002
_exptl_absorpt_correction_T_max  0.74580
_exptl_absorpt_correction_T_min  0.67933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3558
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         15387
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                11260
_reflns_number_total             15387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00263j2.cif
_cod_data_source_block           Tb-p21c
_cod_depositor_comments
'Adding full bibliography for 7219688--7219700.cif.'
_cod_original_formula_sum        'C79.50 H71.5 N3.50 O24 Tb2'
_cod_database_code               7219694
_chemical_oxdiff_formula         C30H30O6N2Tb2
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_submission_special_instructions 'No special instructions were received'