Tetranuclear and Pentanuclear Compounds of the Rare-Earth Metals: Synthesis and Magnetism.
Yadav, Munendra; Mondal, Abhishake; Mereacre, Valeriu; Jana, Salil Kumar; Powell, Annie K.; Roesky, Peter W.; Inorganic chemistry 54 (2015) 7846–7856; doi:10.1021/acs.inorgchem.5b00899

data_4344029
_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
;
 Tetranuclear and Pentanuclear Compounds of the Rare-Earth Metals:
 Synthesis and Magnetism.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7846
_journal_page_last               7856
_journal_paper_doi               10.1021/acs.inorgchem.5b00899
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'C72 H87 Dy4 N4 O19, 3(C2 H6 O), 2(C H4 O), N O3'
_chemical_formula_sum            'C80 H113 Dy4 N5 O27'
_chemical_formula_weight         2225.76
_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   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.154(6)
_cell_length_b                   11.549(2)
_cell_length_c                   24.197(5)
_cell_measurement_reflns_used    40597
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.40
_cell_measurement_theta_min      1.95
_cell_volume                     8706(3)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  'X-STEP32, Microsoft Word'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44012
_diffrn_reflns_point_group_measured_fraction_full 0.864
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.113
_diffrn_reflns_theta_min         1.683
_exptl_absorpt_coefficient_mu    3.472
_exptl_absorpt_correction_T_max  0.7279
_exptl_absorpt_correction_T_min  0.4336
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       plate
_exptl_crystal_F_000             4416
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.652
_refine_diff_density_min         -1.899
_refine_diff_density_rms         0.257
_refine_ls_abs_structure_details
;
 Flack x determined using 3406 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.014(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         14746
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0816P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.683
_reflns_friedel_fraction_full    0.724
_reflns_friedel_fraction_max     0.709
_reflns_number_gt                11260
_reflns_number_total             14746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00899_si_004.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4344028--4344031.cif.'
_cod_database_code               4344029
_shelxl_version_number           2013-2
_shelx_res_checksum              20133
_shelx_hkl_checksum              4211