Highly pH-dependent synthesis of two novel three-dimensional dysprosium complexes with interesting magnetic and luminescence properties
Zhang, Lina; Lu, Shuting; Zhang, Chao; Du, Chenxia; Hou, Hongwei; CrystEngComm 17 (2015) 846–; doi:10.1039/C4CE02023E

data_7218894
_publ_section_title
;
 Highly pH-dependent synthesis of two novel three-dimensional dysprosium
 complexes with interesting magnetic and luminescence properties
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              846
_journal_paper_doi               10.1039/C4CE02023E
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C75 H60 Dy2 N2 O22, 3(C3 H7 N O), O'
_chemical_formula_sum            'C84 H83 Dy2 N5 O26'
_chemical_formula_weight         1903.54
_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             2014-10-26
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  Olex2 1.2
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_cell_angle_beta                 90.00
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_cell_length_a                   19.1237(3)
_cell_length_b                   14.4603(2)
_cell_length_c                   30.6247(4)
_cell_measurement_reflns_used    9085
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      29.1774
_cell_measurement_theta_min      3.0785
_cell_volume                     8468.8(2)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics
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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 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
  1 omega   54.00   92.00   0.5000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000  150.0000 76

  2 omega  -38.00   79.00   0.5000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885    0.0000  -60.0000 234
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0158706000
_diffrn_orient_matrix_UB_12      0.0443468000
_diffrn_orient_matrix_UB_13      0.0000498000
_diffrn_orient_matrix_UB_21      0.0249091000
_diffrn_orient_matrix_UB_22      -0.0154826000
_diffrn_orient_matrix_UB_23      -0.0155253000
_diffrn_orient_matrix_UB_31      -0.0224403000
_diffrn_orient_matrix_UB_32      0.0141450000
_diffrn_orient_matrix_UB_33      -0.0171823000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -14
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_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            24916
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.08
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.831
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1015
_refine_ls_number_reflns         14672
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+6.8098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                13436
_reflns_number_total             14672
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02023e2.cif
_cod_data_source_block           dy-pna21
_cod_depositor_comments
'Adding full bibliography for 7218893--7218894.cif.'
_cod_database_code               7218894
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32