Synthesis and characterization of self-assembled inorganic‒organic hybrid arsenotungstates
Parbhakar, Swati; Kaushik, Reetam; Hussain, Firasat; Acta Crystallographica Section C Structural Chemistry 74 (2018) –; doi:10.1107/S2053229618014171

data_2021396
_publ_section_title
;
 Synthesis and characterization of self-assembled inorganic--organic
 hybrid arsenotungstates
;
_journal_coeditor_code           JR3013
_journal_issue                   12
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229618014171
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
;
K2 {[Cu2 (H2 O) (C12 H8 N2)2 (C2 H3 O2)2]4 [Eu2 (H2 O)2 (C2 H3 O2)2 
(As W11 O39)2]}, 24H2 O1
;
_chemical_formula_moiety
'0.5(C232 H174 As4 Cu16 Er4 K4 N32 O224 W44), 16(O)'
_chemical_formula_sum            'C116 H87 As2 Cu8 Er2 K2 N16 O128 W22'
_chemical_formula_weight         8868.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-02
_audit_creation_method
;
OLEX2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.273(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.581(2)
_cell_length_b                   14.1638(6)
_cell_length_c                   48.299(3)
_cell_measurement_reflns_used    5360
_cell_measurement_temperature    140(20)
_cell_measurement_theta_max      24.4860
_cell_measurement_theta_min      2.8940
_cell_volume                     19865(2)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2013)
;
_computing_molecular_graphics
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OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
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OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2004 (Burla <i>et al.</i>,  2005)
;
_diffrn_ambient_temperature      140(20)
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Agulent Xcalibur Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2474
_diffrn_reflns_av_unetI/netI     0.2009
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            126680
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         2.876
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.829
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    2.965
_exptl_crystal_description       Block
_exptl_crystal_F_000             16076
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.758
_refine_diff_density_min         -2.333
_refine_diff_density_rms         0.502
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         18853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1765
_refine_ls_R_factor_gt           0.0872
_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^)+(0.0242P)^2^+52.5653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9768
_reflns_number_total             18853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3013sup1.cif
_cod_data_source_block           fhsp25c
_cod_database_code               2021396
_publcif_datablock.id            {4d226853-2d58-4010-aae5-c394cbc05916}
_shelx_shelxl_version_number     2017/1
_exptl_absorpt_special_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H1AA(0.5) K1(0.66666) K2(0.33333) O7AA(0.5) O8AA(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46)
3.b Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C1AA(H1AA,H1AB,H1AC), C56(H56A,H56B,
 H56C)
;
_shelx_res_checksum              39122
_shelx_hkl_checksum              9018
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2021396