H-shaped oxalate-bridging lanthanoid-incorporated arsenotungstates.
Chen, Hanhan; Xiao, Zikang; Yan, Bing; Wu, Hechen; Ma, Pengtao; Wang, Jingping; Niu, Jingyang; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15731–15738; doi:10.1039/d0dt02792h

data_7705669
_publ_section_title
;
 H-shaped oxalate-bridging lanthanoid-incorporated arsenotungstates.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15731
_journal_page_last               15738
_journal_paper_doi               10.1039/d0dt02792h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'K17Na2H5, 2(Sm(As2W19O67H2O) 2(H2O) (C2O4)), 56(H2O)'
_chemical_formula_sum            'C2 H129 As4 K17 Na2 O204 Sm2 W38'
_chemical_formula_weight         11714.9
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-05 deposited with the CCDC.	2020-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                67.218(2)
_cell_angle_beta                 81.116(2)
_cell_angle_gamma                79.915(2)
_cell_formula_units_Z            1
_cell_length_a                   12.2892(5)
_cell_length_b                   18.5454(9)
_cell_length_c                   22.9794(11)
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.44
_cell_volume                     4732.3(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.98
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            53152
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         2.194
_diffrn_source_type              Microfocus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.792
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.2957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1440 before and 0.0818 after correction. The Ratio of minimum to maximum transmission is 0.3963. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.065
_exptl_crystal_description       block
_exptl_crystal_F_000             5057
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.542
_refine_diff_density_min         -2.908
_refine_diff_density_rms         0.462
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         16793
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0350P)^2^+328.1932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14185
_reflns_number_total             16793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02792h2.cif
_cod_data_source_block           2018538
_cod_depositor_comments
'Adding full bibliography for 7705668--7705670.cif.'
_cod_database_code               7705669
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.171
_shelx_estimated_absorpt_t_min   0.095
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(O43) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O50)
\\sim Ueq, Uanis(O51) \\sim Ueq, Uanis(O57) \\sim Ueq, Uanis(O29) \\sim Ueq,
Uanis(O34) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O65) \\sim Ueq, Uanis(O66)
\\sim Ueq, Uanis(O46) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O18) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
2. Others
 Fixed Sof: W13(0.95) K8(0.5) K9(0.5) K10(0.5) O14W(0.5) O16W(0.5) O21W(0.5)
 O22W(0.5) O24W(0.5) O25W(0.5) O29W(0.5) O33W(0.5) O34W(0.5) O35W(0.5)
 O36W(0.5) O37W(0.5) O38W(0.5) O40W(0.5) O41W(0.5) O39W(0.5) W13B(0.05)
;
_shelx_res_checksum              97397
_shelx_fab_checksum              19322
_olex2_submission_special_instructions 'No special instructions were received'