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_2021391
_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_moiety
'C116 H90.67 As2 Cu8 Eu2 K2 N16 O110 W22, 7.5(O)'
_chemical_formula_sum            'C116 H90.67 As2 Cu8 Eu2 K2 N16 O117.5 W22'
_chemical_formula_weight         8673.69
_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             2018-11-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.836(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.5449(13)
_cell_length_b                   14.2507(5)
_cell_length_c                   48.6187(17)
_cell_measurement_reflns_used    11692
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1960
_cell_measurement_theta_min      3.1500
_cell_volume                     20145.9(14)
_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  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT2014 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9853
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -80.00 -54.00   1.00   12.00    --  -16.10   0.00-180.00   26
  2  \w    -86.00   6.00   1.00   12.00    --  -16.10 -77.00  30.00   92
  3  \w    -49.00  53.00   1.00   12.00    --  -16.10   0.00-180.00  102
  4  \w    -80.00   9.00   1.00   12.00    --  -16.10 -38.00 150.00   89
  5  \w      7.00  56.00   1.00   12.00    --  -16.10  38.00 -30.00   49
  6  \w    -25.00  23.00   1.00   12.00    --  -16.10 -99.00 -90.00   48
  7  \w    -50.00  28.00   1.00   12.00    --   20.31 -77.00 -90.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0117396000
_diffrn_orient_matrix_UB_12      -0.0225683000
_diffrn_orient_matrix_UB_13      -0.0132065000
_diffrn_orient_matrix_UB_21      -0.0006317000
_diffrn_orient_matrix_UB_22      -0.0422487000
_diffrn_orient_matrix_UB_23      0.0075803000
_diffrn_orient_matrix_UB_31      -0.0213704000
_diffrn_orient_matrix_UB_32      0.0136012000
_diffrn_orient_matrix_UB_33      0.0016811000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1090
_diffrn_reflns_av_unetI/netI     0.1040
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            83314
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         2.802
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.426
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    2.860
_exptl_crystal_description       Block
_exptl_crystal_F_000             15715
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.777
_refine_diff_density_min         -1.558
_refine_diff_density_rms         0.394
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     995
_refine_ls_number_reflns         18907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0554P)^2^+694.6223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12701
_reflns_number_total             18907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3013sup1.cif
_cod_data_source_block           fhsp17b
_cod_original_formula_sum        'C116 H90.67 As2 Cu8 Eu2 K2 N16 O117.50 W22'
_cod_database_code               2021391
_publcif_datablock.id            {229a5307-5d7d-4b6d-bcb8-2d7f0885f29d}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu As W O Eu C N Rb Cl H'
_chemical_oxdiff_usercomment     29-06-2016
_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 98.21
_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: H54C(0.3336) K1(0.6664) K2(0.3336) O53(0.5) O54(0.25) O61(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B)
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), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,
 H58C)
;
_shelx_res_checksum              9776
_shelx_hkl_checksum              50553
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 9.296
_oxdiff_exptl_absorpt_empirical_full_min 0.603