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_4341105
_publ_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT)
      Institut fuer Anorganische Chemie
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_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         '(C40 H40 Y1 N4 O16),(H2 O),(c2 H8 N O)'
_chemical_formula_sum            'C42 H50 N5 O18 Y'
_chemical_formula_weight         1001.78
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4777)
;
_cell_angle_alpha                90
_cell_angle_beta                 134.97(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.955(5)
_cell_length_b                   14.600(3)
_cell_length_c                   16.930(3)
_cell_measurement_reflns_used    5680
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      1.84
_cell_volume                     4189(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0818
_diffrn_reflns_av_unetI/netI     0.1183
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11960
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.508
_diffrn_reflns_theta_min         1.842
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_T_max  0.9148
_exptl_absorpt_correction_T_min  0.8387
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.093
_refine_diff_density_max         1.614
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         3886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0688P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2483
_reflns_number_total             3886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5014957_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4341104--4341108.cif.'
_cod_original_cell_volume        4189(2)
_cod_database_code               4341105
_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, All C(H,H,H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H34D(0.5) H34C(0.5) H34B(0.5) H34A(0.5) H22D(0.5) H22C(0.5)
 H22A(0.5) H22B(0.5) O26(0.5) H26(0.5) O48(0.5) H48(0.5) O50(0.5) H50(0.5)
 N1(0.5) H1C(0.5) H1A(0.5) H1B(0.5) O1(0.5) H1(0.5) O8(0.5) H8(0.5) O2(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C34(H34D,H34C), C34(H34B,H34A), C22(H22D,H22C), C22(H22A,H22B), C35(H35A,
 H35B), C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C36(H36), C4(H4), C13(H13), C30(H30), C5(H5), C42(H42), C3(H3)
3.c Idealised Me refined as rotating group:
 N1(H1C,H1A,H1B)
3.d Idealised tetrahedral OH refined as rotating group:
 O26(H26), O48(H48), O50(H50), O1(H1), O8(H8)
;
_shelx_res_checksum              59283
_shelx_hkl_checksum              62704
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'