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_7219698
_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_absolute_configuration ad
_chemical_formula_moiety         'C75 H54 Ho2 N2 O22, 3(C3 H7 N O), O'
_chemical_formula_sum            'C84 H83 Ho2 N5 O26'
_chemical_formula_weight         1908.35
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-12
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  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
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_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0994(2)
_cell_length_b                   14.41797(17)
_cell_length_c                   30.5930(5)
_cell_measurement_reflns_used    10690
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      29.1462
_cell_measurement_theta_min      3.0089
_cell_volume                     8424.53(19)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega   -2.00   41.00   0.5000   12.1600
omega____ theta____ kappa____ phi______ frames
    -      -17.1323   57.0000    0.0000 86

  2 omega   21.00   86.00   0.5000   12.1600
omega____ theta____ kappa____ phi______ frames
    -       19.7885   37.0000   90.0000 130

  3 omega   58.00   96.00   0.5000   12.1600
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000    0.0000 76
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0300853000
_diffrn_orient_matrix_UB_12      -0.0287420000
_diffrn_orient_matrix_UB_13      0.0011007000
_diffrn_orient_matrix_UB_21      -0.0080292000
_diffrn_orient_matrix_UB_22      -0.0183639000
_diffrn_orient_matrix_UB_23      -0.0209240000
_diffrn_orient_matrix_UB_31      0.0202192000
_diffrn_orient_matrix_UB_32      0.0354552000
_diffrn_orient_matrix_UB_33      -0.0099386000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22596
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         3.12
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.945
_exptl_absorpt_correction_T_max  0.82900
_exptl_absorpt_correction_T_min  0.69352
_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    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1026
_refine_ls_number_reflns         12351
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+9.6142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                11114
_reflns_number_total             12351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00263j2.cif
_cod_data_source_block           Ho-pna21
_cod_depositor_comments
'Adding full bibliography for 7219688--7219700.cif.'
_cod_original_cell_volume        8424.51(19)
_cod_database_code               7219698
_chemical_oxdiff_formula         C30H3O6N2Ho2
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32