Double-malate bridging tri-lanthanoid cluster encapsulated arsenotungstates: syntheses, structures, luminescence and magnetic properties.
Ma, Pengtao; Wan, Rong; Si, Yanan; Hu, Feng; Wang, Yueyan; Niu, Jingyang; Wang, Jingping; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11514–11523; doi:10.1039/c5dt01323b

data_7035310
_publ_section_title
;
 Double-malate bridging tri-lanthanoid cluster encapsulated
 arsenotungstates: syntheses, structures, luminescence and magnetic
 properties.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11514
_journal_page_last               11523
_journal_paper_doi               10.1039/c5dt01323b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         '0.5(C16 H12 As8 K40 Li4 O360 Tb12 W76), O'
_chemical_formula_sum            'C8 H74 As4 K20 Li2 O181 Tb6 W38'
_chemical_formula_weight         12102.05
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-05 deposited with the CCDC.
2015-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.785(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.924(3)
_cell_length_b                   25.288(4)
_cell_length_c                   22.707(4)
_cell_measurement_reflns_used    8970
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.26
_cell_volume                     11077(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1049
_diffrn_reflns_av_unetI/netI     0.1206
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56070
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.87
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.588
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.1827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1787 before and 0.0779 after correction.
The Ratio of minimum to maximum transmission is 0.2450.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10580
_exptl_crystal_preparation       'Magnetic properties, Luminescent'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         5.578
_refine_diff_density_min         -3.631
_refine_diff_density_rms         0.568
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         19474
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1099P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.2029
_reflns_number_gt                12652
_reflns_number_total             19474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01323b2.cif
_cod_data_source_block           1043920
_cod_depositor_comments
'Adding full bibliography for 7035309--7035313.cif.'
_cod_database_code               7035310
_audit_block_doi                 10.5517/cc1418v9
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O30)
\\sim Ueq, Uanis(O37) \\sim Ueq, Uanis(O44) \\sim Ueq, Uanis(O58) \\sim Ueq,
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O15) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O49) \\sim Ueq, Uanis(O64)
\\sim Ueq, Uanis(O57) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: K3(0.5) K4(0.5) K5(0.5) K6(0.5) K7(0.5) K8(0.5) K9(0.5) K10(0.5)
 K11(0.5) K12(0.5) K13(0.5) K14(0.5) K15(0.5) K16(0.25) K17(0.25) K18(0.25)
 K19(0.25) K20(0.25) K21(0.25) O10W(0.5) O11W(0.5) O12W(0.5) O13W(0.5)
 O14W(0.5) O15W(0.5) O16W(0.5) O17W(0.5) O18W(0.5) O19W(0.5) O20W(0.5)
 O21W(0.5) O22W(0.5) O23W(0.5) O24W(0.5)
 Fixed Uiso: K15(0.15762) O9W(0.11532) O20W(0.10311) O23W(0.11879) O24W(0.11649)
4.a Ternary CH refined with riding coordinates:
 C2(H2)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
;