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_2021395
_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 [Ho2 (H2 O)2 (C2 H3 O2)2 
(As W11 O39)2]}, 24H2 O1
;
_chemical_formula_moiety         'C116 H94 As2 Cu8 Ho2 K2 N16 O112 W22, 16(O)'
_chemical_formula_sum            'C116 H94 As2 Cu8 Ho2 K2 N16 O128 W22'
_chemical_formula_weight         8870.99
_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
_atom_sites_solution_primary     direct
_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                 108.169(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.4802(7)
_cell_length_b                   14.1130(3)
_cell_length_c                   48.1160(13)
_cell_measurement_reflns_used    19107
_cell_measurement_temperature    172(60)
_cell_measurement_theta_max      28.2540
_cell_measurement_theta_min      2.7990
_cell_volume                     19665.9(9)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2013)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
ShelXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      172(60)
_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  0.1059
_diffrn_reflns_av_unetI/netI     0.0857
_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            123225
_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         2.813
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.930
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    2.996
_exptl_crystal_description       Block
_exptl_crystal_F_000             16096
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.658
_refine_diff_density_min         -1.611
_refine_diff_density_rms         0.323
_refine_ls_extinction_coef       0.0000015(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2017 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         18640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0273P)^2^+248.0512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13506
_reflns_number_total             18640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3013sup1.cif
_cod_data_source_block           fhsp24d
_cod_database_code               2021395
_publcif_datablock.id            {e6b767e9-a7cc-4763-9a50-737004035323}
_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: K1(0.6) K0AA(0.4)
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), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              14385
_shelx_hkl_checksum              44479
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2021395