Mononuclear and tetranuclear compounds of yttrium and dysprosium ligated by a salicylic schiff-base derivative: synthesis, photoluminescence, and magnetism.
Yadav, Munendra; Mereacre, Valeriu; Lebedkin, Sergei; Kappes, Manfred M.; Powell, Annie K.; Roesky, Peter W.; Inorganic chemistry 54 (2015) 773–781; doi:10.1021/ic5014957

data_4341104
_publ_section_title
;
 Mononuclear and tetranuclear compounds of yttrium and dysprosium ligated
 by a salicylic schiff-base derivative: synthesis, photoluminescence, and
 magnetism.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              773
_journal_page_last               781
_journal_paper_doi               10.1021/ic5014957
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'C100 H88 Dy4 N10 O40, 3(C H4 O), 2(C0.5 O0.5), 2(O)'
_chemical_formula_sum            'C104 H118 Dy4 N10 O46'
_chemical_formula_weight         2894.08
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4779)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.884(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6078(4)
_cell_length_b                   15.2410(6)
_cell_length_c                   25.4038(8)
_cell_measurement_temperature    100(2)
_cell_volume                     5635.3(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0989
_diffrn_reflns_av_unetI/netI     0.1002
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26018
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.092
_diffrn_reflns_theta_min         1.553
_exptl_absorpt_coefficient_mu    2.717
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_F_000             2888
_refine_diff_density_max         1.821
_refine_diff_density_min         -1.997
_refine_diff_density_rms         0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         10994
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0916P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7707
_reflns_number_total             10994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5014957_si_006.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4341104--4341108.cif.'
_cod_database_code               4341104
_shelxl_version_number           2013-2
_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 O(H) groups
2. Restrained distances
 O20-H20
 0.85 with sigma of 0.01
 C50-H20
 1.900853 with sigma of 0.02
 Dy2-H20
 2.874253 with sigma of 0.02
3. Others
 Fixed Sof: C51(0.5) C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) H47A(0.5)
 H47B(0.5) C48A(0.5) H48A(0.5) H48B(0.5) C48B(0.5) H48C(0.5) H48D(0.5)
 O21B(0.25) O23(0.5) H23A(0.5) O21A(0.25) O17A(0.6) H17A(0.6) O17B(0.4)
 H17B(0.4)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C19(H19A,H19B), C20(H20A,H20B), C29(H29A,H29B),
 C37(H37A,H37B), C38(H38A,H38B), C47(H47A,H47B), C48A(H48A,H48B), C48B(H48C,
 H48D), C50(H50A,H50B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C13(H13), C14(H14), C15(H15), C18(H18),
 C24(H24), C25(H25), C28(H28), C32(H32), C33(H33), C34(H34), C36(H36), C41(H41),
  C42(H42), C43(H43), C46(H46)
4.c Aromatic/amide H refined with riding coordinates and stretchable bonds:
 C23(H23)
4.d Idealised Me refined with riding coordinates:
 C53(H53A,H53B,H53C)
4.e Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C)
4.f Idealised tetrahedral OH refined with riding coordinates:
 O23(H23A), O13(H13A), O17B(H17B)
4.g Idealised tetrahedral OH refined as rotating group:
 O22(H22), O4(H4A), O8(H8A), O17A(H17A)
;
_shelx_res_checksum              84234
_shelx_hkl_checksum              5554
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'