Realgar as a Building Block for Lanthanide Clusters: Encapsulation of a Copper Cluster by a Lanthanide Cluster.
Arleth, Nicholas; Bestgen, Sebastian; Gamer, Michael T.; Roesky, Peter W.; Journal of the American Chemical Society 136 (2014) 14023–; doi:10.1021/ja508880z

data_4122659
_publ_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT), CS
      Institut fuer Anorganische Chemie (AOC)
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_publ_section_title
;
 Realgar as a Building Block for Lanthanide Clusters: Encapsulation of a
 Copper Cluster by a Lanthanide Cluster.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14023
_journal_paper_doi               10.1021/ja508880z
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C84 H148 Cu4 O4 S6 Sm4, 2(C4 H8 O)'
_chemical_formula_sum            'C92 H164 Cu4 O6 S6 Sm4'
_chemical_formula_weight         2414.14
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.2460(7)
_cell_length_b                   38.9864(6)
_cell_length_c                   13.6966(3)
_cell_measurement_reflns_used    53420
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      30.73
_cell_measurement_theta_min      1.51
_cell_volume                     19888.7(7)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED & LANA, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Diamond 2/3, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'MS Word, Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Dectris Pilatus 100k'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41116
_diffrn_reflns_point_group_measured_fraction_full 0.880
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.247
_diffrn_reflns_theta_min         1.512
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_type              'Xenocs Genix3D microfocus'
_exptl_absorpt_coefficient_mu    3.333
_exptl_absorpt_correction_T_max  0.9945
_exptl_absorpt_correction_T_min  0.9688
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & LANA'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       plank
_exptl_crystal_F_000             9792
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.104
_refine_diff_density_max         1.113
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.004(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7938
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.682
_reflns_Friedel_fraction_full    0.748
_reflns_Friedel_fraction_max     0.748
_reflns_number_gt                7413
_reflns_number_total             7938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508880z_si_006.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4122659--4122664.cif.'
_cod_database_code               4122659
_shelxl_version_number           2014-3
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: H36A(0.5) H36B(0.5) H36C(0.5) H36D(0.5) H38A(0.5) H38B(0.5)
 H38C(0.5) H38D(0.5) C37A(0.5) H37A(0.5) H37B(0.5) C37B(0.5) H37C(0.5) H37D(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C36(H36C,H36D), C38(H38A,H38B), C38(H38C,H38D), C35(H35A,
 H35B), C39(H39A,H39B), C41(H41A,H41B), C40(H40A,H40B), C42(H42A,H42B),
 C45(H45A,H45B), C43(H43A,H43B), C44(H44A,H44B), C46(H46A,H46B), C37A(H37A,
 H37B), C37B(H37C,H37D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C19(H19), C5(H5), C22(H22)
4.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C9(H9A,H9B,H9C), C25(H25A,H25B,H25C), C33(H33A,H33B,
 H33C), C30(H30A,H30B,H30C), C8(H8A,H8B,H8C), C29(H29A,H29B,H29C), C7(H7A,H7B,
 H7C), C11(H11A,H11B,H11C), C24(H24A,H24B,H24C), C17(H17A,H17B,H17C), C28(H28A,
 H28B,H28C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C26(H26A,H26B,H26C),
 C32(H32A,H32B,H32C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              9913
_shelx_hkl_checksum              71188
_olex2_submission_special_instructions 'No special instructions were received'