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_4122661
_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         'C48 H76 As3 O2 S6 Yb3, C4 H8 O'
_chemical_formula_sum            'C52 H84 As3 O3 S6 Yb3'
_chemical_formula_weight         1693.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                85.64(3)
_cell_angle_beta                 87.33(3)
_cell_angle_gamma                69.09(3)
_cell_formula_units_Z            2
_cell_length_a                   13.009(3)
_cell_length_b                   13.399(3)
_cell_length_c                   19.680(4)
_cell_measurement_reflns_used    31783
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      1.63
_cell_volume                     3194.5(14)
_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      150.15
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_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  0.1169
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30869
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.782
_diffrn_reflns_theta_min         1.630
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    6.129
_exptl_absorpt_correction_T_max  0.6682
_exptl_absorpt_correction_T_min  0.3245
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       plate
_exptl_crystal_F_000             1650
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.077
_refine_diff_density_max         3.774
_refine_diff_density_min         -2.695
_refine_diff_density_rms         0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         13467
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0682
_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^)+(0.1127P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1675
_refine_ls_wR_factor_ref         0.1776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10520
_reflns_number_total             13467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508880z_si_003.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4122659--4122664.cif.'
_cod_original_cell_volume        3194.7(13)
_cod_database_code               4122661
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C47A-C46A \\sim C47B-C46B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Same fragment restrains
{O1, C41, C42, C43, C44}
as
{O4, C53, C54, C55, C56}
{O1, C41, C42, C43, C44}
as
{O3, C49, C50, C51, C52}
5. Others
 Fixed Sof: O2A(0.66667) O2B(0.33333) C21A(0.5) C21B(0.5) C22A(0.5) C22B(0.5)
 C23A(0.5) C23B(0.5) C24A(0.5) C24B(0.5) C25A(0.5) C25B(0.5) C26A(0.5)
 H26A(0.5) H26B(0.5) H26C(0.5) C26B(0.5) H26D(0.5) H26E(0.5) H26F(0.5)
 C27A(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C27B(0.5) H27D(0.5) H27E(0.5)
 H27F(0.5) C28A(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C28B(0.5) H28D(0.5)
 H28E(0.5) H28F(0.5) C29A(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C29B(0.5)
 H29D(0.5) H29E(0.5) H29F(0.5) C30A(0.5) H30A(0.5) H30B(0.5) H30C(0.5)
 C30B(0.5) H30D(0.5) H30E(0.5) H30F(0.5) C45A(0.66667) H45A(0.66667)
 H45B(0.66667) C45B(0.33333) H45C(0.33333) H45D(0.33333) C46A(0.66667)
 H46A(0.66667) H46B(0.66667) C46B(0.33333) H46C(0.33333) H46D(0.33333)
 C47A(0.66667) H47A(0.66667) H47B(0.66667) C47B(0.33333) H47C(0.33333)
 H47D(0.33333) C48A(0.66667) H48A(0.66667) H48B(0.66667) C48B(0.33333)
 H48C(0.33333) H48D(0.33333) O4(0.5) C53(0.5) H53A(0.5) H53B(0.5) C54(0.5)
 H54A(0.5) H54B(0.5) C55(0.5) H55A(0.5) H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5)
 O3(0.5) C49(0.5) H49A(0.5) H49B(0.5) C50(0.5) H50A(0.5) H50B(0.5) C51(0.5)
 H51A(0.5) H51B(0.5) C52(0.5) H52A(0.5) H52B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45A(H45A,
 H45B), C45B(H45C,H45D), C46A(H46A,H46B), C46B(H46C,H46D), C47A(H47A,H47B),
 C47B(H47C,H47D), C48A(H48A,H48B), C48B(H48C,H48D), C53(H53A,H53B), C54(H54A,
 H54B), C55(H55A,H55B), C56(H56A,H56B), C49(H49A,H49B), C50(H50A,H50B),
 C51(H51A,H51B), C52(H52A,H52B)
6.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), C26A(H26A,H26B,H26C), C26B(H26D,H26E,
 H26F), C27A(H27A,H27B,H27C), C27B(H27D,H27E,H27F), C28A(H28A,H28B,H28C),
 C28B(H28D,H28E,H28F), C29A(H29A,H29B,H29C), C29B(H29D,H29E,H29F), C30A(H30A,
 H30B,H30C), C30B(H30D,H30E,H30F), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              95473
_shelx_hkl_checksum              84162
_olex2_submission_special_instructions 'No special instructions were received'