Organically templated metal sulfate-oxalates: Solvent-free synthesis, crystal structure, and proton conduction
Zhang, Ying; Lin, Longzhen; Zeng, Hongmei; Zou, Guohong; Lin, Zhien; Journal of Solid State Chemistry 276 (2019) 1–5; doi:10.1016/j.jssc.2019.04.031

data_1563785
_publ_section_title
;
 Organically templated metal sulfate-oxalates: Solvent-free synthesis,
 crystal structure, and proton conduction
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              1
_journal_page_last               5
_journal_paper_doi               10.1016/j.jssc.2019.04.031
_journal_volume                  276
_journal_year                    2019
_chemical_formula_moiety         'C2 O9 S V, C5 H14 N2'
_chemical_formula_sum            'C7 H14 N2 O9 S V'
_chemical_formula_weight         353.20
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                77.130(5)
_cell_angle_beta                 76.207(5)
_cell_angle_gamma                82.987(5)
_cell_formula_units_Z            2
_cell_length_a                   6.2031(4)
_cell_length_b                   8.6599(4)
_cell_length_c                   12.1853(7)
_cell_measurement_reflns_used    3759
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.2140
_cell_measurement_theta_min      5.2310
_cell_volume                     618.08(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      air
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega   23.00   90.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000   60.0000 67

  2 omega   20.00  104.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000   90.0000 84

  3 omega   20.00  104.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000    0.0000 84

  4 omega   20.00  104.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  -30.0000 84

  5 omega  -31.00   53.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000  120.0000 84

  6 omega    1.00   75.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000   90.0000 74

  7 omega  -33.00   55.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000 -180.0000 88

  8 omega   23.00   90.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000  -90.0000 67

  9 omega   39.00  109.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 70

 10 omega   40.00   98.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  150.0000 58

 11 omega   38.00  116.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -60.0000 78

 12 omega   38.00  116.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  150.0000 78

 13 omega   41.00  126.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  -90.0000 85

 14 omega  100.00  178.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000    0.0000 78

 15 omega   40.00   98.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 58

 16 omega   37.00  146.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000 -120.0000 109

 17 omega   91.00  176.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  150.0000 85

 18 omega   38.00   91.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

 19 omega   41.00  126.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000    0.0000 85

 20 omega   70.00  178.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000   90.0000 108

 21 omega   39.00  109.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -180.0000 70

 22 omega   38.00   91.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 53

 23 omega  100.00  178.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -60.0000 78

 24 omega  -35.00   66.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -19.0000  -90.0000 101

 25 omega   10.00  104.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000 -150.0000 94

 26 omega   20.00  104.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  -90.0000 84

 27 omega   10.00  104.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000    0.0000 94

 28 omega  -33.00   55.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000    0.0000 88

 29 omega   20.00  104.00   1.0000    5.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  150.0000 84

 30 omega   70.00  178.00   1.0000   22.6100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -60.0000 108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1378753000
_diffrn_orient_matrix_UB_12      0.0582027000
_diffrn_orient_matrix_UB_13      -0.1224414000
_diffrn_orient_matrix_UB_21      0.2152526000
_diffrn_orient_matrix_UB_22      -0.0373648000
_diffrn_orient_matrix_UB_23      0.0460515000
_diffrn_orient_matrix_UB_31      0.0200737000
_diffrn_orient_matrix_UB_32      -0.1693902000
_diffrn_orient_matrix_UB_33      -0.0233949000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6715
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         5.253
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.798
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             362
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_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     182
_refine_ls_number_reflns         2216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+0.1135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2068
_reflns_number_total             2216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2019-276-1.CIF
_cod_data_source_block           1
_cod_database_code               1563785
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_shelxl_version_number     2014/7