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_4344030
_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         'C136 H124 Dy5 N6 O23, 4(C H4 O)'
_chemical_formula_sum            'C140 H140 Dy5 N6 O27'
_chemical_formula_weight         3151.13
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.378(6)
_cell_length_b                   29.921(6)
_cell_length_c                   32.547(7)
_cell_measurement_reflns_used    39606
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.52
_cell_measurement_theta_min      1.19
_cell_volume                     26662(10)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.1173
_diffrn_reflns_laue_measured_fraction_full 0.988
_diffrn_reflns_laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            90588
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.252
_diffrn_reflns_theta_min         1.186
_exptl_absorpt_coefficient_mu    2.841
_exptl_absorpt_correction_T_max  0.8009
_exptl_absorpt_correction_T_min  0.6235
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       prism
_exptl_crystal_F_000             12464
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.113
_refine_diff_density_max         1.740
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1599
_refine_ls_number_reflns         23834
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0283P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13704
_reflns_number_total             23834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00899_si_003.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4344028--4344031.cif.'
_cod_original_cell_volume        26662(9)
_cod_database_code               4344030
_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
 O21-H21
 0.87 with sigma of 0.01
 C134-H21
 1.913111 with sigma of 0.02
 Dy1-H21
 2.85712 with sigma of 0.02
3. Others
 Fixed Sof: O22A(0.5) O22B(0.5) C1XA(0.5) H1XA(0.5) C2EA(0.5) H2EA(0.5)
 C36A(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C36B(0.5) H36D(0.5) H36E(0.5)
 H36F(0.5) C37A(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C37B(0.5) H37D(0.5)
 H37E(0.5) H37F(0.5) C38A(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C38B(0.5)
 H38D(0.5) H38E(0.5) H38F(0.5) C60A(0.5) H60A(0.5) H60B(0.5) H60C(0.5)
 C60B(0.5) H60D(0.5) H60E(0.5) H60F(0.5) C61A(0.5) H61A(0.5) H61B(0.5)
 H61C(0.5) C61B(0.5) H61D(0.5) H61E(0.5) H61F(0.5) C62A(0.5) H62A(0.5)
 H62B(0.5) H62C(0.5) C62B(0.5) H62D(0.5) H62E(0.5) H62F(0.5) H68A(0.5) H68(0.5)
 C69(0.5) H69(0.5) C70(0.5) H70(0.5) H71(0.5) H71A(0.5) C88A(0.5) H88A(0.5)
 C88B(0.5) H88B(0.5) C89A(0.5) H89A(0.5) C89B(0.5) H89B(0.5) C90A(0.5)
 H90A(0.5) C90B(0.5) H90B(0.5) C91A(0.5) H91A(0.5) C91B(0.5) H91B(0.5)
 C92A(0.5) H92A(0.5) C92B(0.5) H92B(0.5) H98A(0.5) H98(0.5) C99A(0.5) H99A(0.5)
 C99B(0.5) H99B(0.5) H10A(0.5) H100(0.5) C103(0.5) H103(0.5) C104(0.5)
 H104(0.5) C105(0.5) H105(0.5) C106(0.5) H106(0.5) C107(0.5) H107(0.5)
 C108(0.5) C135(0.5) H13J(0.5) H13K(0.5) H13L(0.5) C203(0.5) H203(0.5)
 C204(0.5) H204(0.5) C205(0.5) H205(0.5) C206(0.5) H206(0.5) C207(0.5)
 H207(0.5) C208(0.5) C235(0.5) H23B(0.5) H23C(0.5) H23D(0.5) O26A(0.5)
 C239(0.5) O27A(0.5) C140(0.5) O26B(0.5) C139(0.5) O27B(0.5) C240(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1XA(H1XA), C2(H2), C2EA(H2EA), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9),
 C15(H15), C18(H18), C20(H20A), C21(H21A), C22(H22), C23(H23A), C26(H26),
 C27(H27), C28(H28), C29(H29), C31(H31), C33(H33), C39(H39), C42(H42), C44(H44),
  C45(H45), C46(H46), C47(H47), C50(H50), C51(H51), C52(H52), C53(H53),
 C55(H55), C57(H57), C63(H63), C66(H66), C68(H68A), C68(H68), C69(H69),
 C70(H70), C71(H71), C71(H71A), C73(H73), C74(H74), C75(H75), C76(H76),
 C77(H77), C80(H80), C83(H83), C84(H84), C85(H85), C86(H86), C87(H87),
 C88A(H88A), C88B(H88B), C89A(H89A), C89B(H89B), C90A(H90A), C90B(H90B),
 C91A(H91A), C91B(H91B), C92A(H92A), C92B(H92B), C95(H95), C98(H98A), C98(H98),
 C99A(H99A), C99B(H99B), C100(H10A), C100(H100), C101(H101), C102(H102),
 C103(H103), C104(H104), C105(H105), C106(H106), C107(H107), C110(H110),
 C113(H113), C114(H114), C115(H115), C116(H116), C117(H117), C118(H118),
 C119(H119), C120(H120), C121(H121), C122(H122), C125(H125), C128(H128),
 C129(H129), C130(H130), C131(H131), C132(H132), C203(H203), C204(H204),
 C205(H205), C206(H206), C207(H207)
4.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C36A(H36A,H36B,
 H36C), C36B(H36D,H36E,H36F), C37A(H37A,H37B,H37C), C37B(H37D,H37E,H37F),
 C38A(H38A,H38B,H38C), C38B(H38D,H38E,H38F), C60A(H60A,H60B,H60C), C60B(H60D,
 H60E,H60F), C61A(H61A,H61B,H61C), C61B(H61D,H61E,H61F), C62A(H62A,H62B,H62C),
 C62B(H62D,H62E,H62F), C133(H13D,H13E,H13F), C134(H13G,H13H,H13I), C135(H13J,
 H13K,H13L), C136(H13M,H13N,H13O), C235(H23B,H23C,H23D), C138(H13P,H13Q,H13R),
 C137(H13S,H13T,H13U)
4.c Idealised tetrahedral OH refined with riding coordinates:
 O24(H24)
4.d Idealised tetrahedral OH refined as rotating group:
 O25(H25)
;
_shelx_res_checksum              94605
_shelx_hkl_checksum              85229
_olex2_submission_special_instructions 'No special instructions were received'