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_4122660
_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         'C82 H129 As3 O3 S7 Sm4, C4 H8 O'
_chemical_formula_sum            'C86 H137 As3 O4 S7 Sm4'
_chemical_formula_weight         2285.53
_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   geom
_audit_creation_date             2014-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.652(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1249(4)
_cell_length_b                   25.8707(4)
_cell_length_c                   20.4267(4)
_cell_measurement_reflns_used    94622
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.64
_cell_measurement_theta_min      1.79
_cell_volume                     9531.6(3)
_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      150
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0304
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            71710
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.104
_diffrn_reflns_theta_min         1.581
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    3.659
_exptl_absorpt_correction_T_max  0.3694
_exptl_absorpt_correction_T_min  0.2406
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       prism
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.518
_exptl_crystal_size_mid          0.434
_exptl_crystal_size_min          0.379
_refine_diff_density_max         1.220
_refine_diff_density_min         -1.408
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     981
_refine_ls_number_reflns         18767
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+16.7564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16967
_reflns_number_total             18767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508880z_si_007.cif
_cod_data_source_block           na84_sq
_cod_depositor_comments
'Adding full bibliography for 4122659--4122664.cif.'
_cod_database_code               4122660
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58)
\\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
3. Others
 Fixed Sof: H76C(0.5) H76D(0.5) H76A(0.5) H76B(0.5) C77B(0.5) H77A(0.5)
 H77B(0.5) H78C(0.5) H78D(0.5) H78A(0.5) H78B(0.5) C77A(0.5) H77C(0.5) H77D(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,
 H75B), C76(H76C,H76D), C76(H76A,H76B), C77B(H77A,H77B), C78(H78C,H78D),
 C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B),
  C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C77A(H77C,
 H77D)
4.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C),
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C70(H70A,H70B,H70C)
;
_shelx_res_checksum              94886
_shelx_hkl_checksum              72972
_shelx_fab_checksum              42403
_olex2_submission_special_instructions 'No special instructions were received'