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_2021392
_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 [Gd2 (H2 O)2 (C2 H3 O2)2 
(As W11 O39)2]}, 22H2 O1
;
_chemical_formula_moiety         'C116 H92 As2 Cu8 Gd2 K2 N16 O110 W22, 16(O)'
_chemical_formula_sum            'C116 H92 As2 Cu8 Gd2 K2 N16 O126 W22'
_chemical_formula_weight         8821.61
_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             2018-05-09
_audit_creation_method
;
OLEX2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.131(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.5038(7)
_cell_length_b                   14.1439(4)
_cell_length_c                   48.2029(12)
_cell_measurement_reflns_used    19211
_cell_measurement_temperature    190(20)
_cell_measurement_theta_max      28.3750
_cell_measurement_theta_min      3.1490
_cell_volume                     19764.2(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)
;
_diffrn_ambient_temperature      190(20)
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -85.00    5.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0952  -57.0000  120.0000 90

  2 omega  -54.00   34.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0952   91.0000   65.2166 88

  3 omega  -71.00    5.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0952  -57.0000    0.0000 76

  4 omega  -36.00   53.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0952   57.0000  -90.0000 89

  5 omega  -21.00   62.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3140  -99.0000    0.0000 83

  6 omega  -42.00   49.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3140  -77.0000 -180.0000 91

  7 omega   -9.00   90.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3140   77.0000  -60.0000 99

  8 omega   -4.00   66.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3140   38.0000  -90.0000 70
;
_diffrn_measurement_device_type  'Agulent Xcalibur Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0126285000
_diffrn_orient_matrix_UB_12      0.0314381000
_diffrn_orient_matrix_UB_13      0.0110609000
_diffrn_orient_matrix_UB_21      0.0051302500
_diffrn_orient_matrix_UB_22      -0.0377561500
_diffrn_orient_matrix_UB_23      0.0102096500
_diffrn_orient_matrix_UB_31      0.0203175000
_diffrn_orient_matrix_UB_32      -0.0101340000
_diffrn_orient_matrix_UB_33      -0.0036363000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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            123422
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.065
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31319
_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             16000
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.977
_refine_diff_density_min         -1.847
_refine_diff_density_rms         0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         18730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0228P)^2^+986.8466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15124
_reflns_number_total             18730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3013sup1.cif
_cod_data_source_block           fhsp21c
_cod_database_code               2021392
_publcif_datablock.id            {3295d2d5-87ac-415a-a35d-89fdd9060950}
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Cu Gd As W o C N Na K'
_chemical_oxdiff_usercomment     22-11-2016
_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.
;
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: K1(0.66667) K2(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B)
3.b 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.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C56(H56A,H56B,H56C), C58(H58A,H58B,
 H58C)
;
_shelx_res_checksum              7625
_shelx_hkl_checksum              83445
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2021392