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_1563786
_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         'C4 H2 Mn2 O13 S, H2 O, C7 H20 N2'
_chemical_formula_sum            'C11 H24 Mn2 N2 O14 S'
_chemical_formula_weight         550.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.6293(3)
_cell_length_b                   15.6671(3)
_cell_length_c                   17.3579(3)
_cell_measurement_reflns_used    4091
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.3550
_cell_measurement_theta_min      4.8650
_cell_volume                     3978.41(13)
_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_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   18.00  106.00   1.0000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421   38.0000  -60.0000 88

  2 omega   18.00  106.00   1.0000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421   38.0000   30.0000 88

  3 omega  -35.00   66.00   1.0000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -19.0000  -30.0000 101

  4 omega   23.00   90.00   1.0000    2.6500
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000 -180.0000 67

  5 omega   38.00   91.00   1.0000   10.6000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

  6 omega   44.00   95.00   1.0000   10.6000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 51

  7 omega   41.00   77.00   1.0000   10.6000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 36

  8 omega  114.00  169.00   1.0000   10.6000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000   90.0000 55

  9 omega   47.00  177.00   1.0000   10.6000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000 -120.0000 130
;
_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      -0.0473024000
_diffrn_orient_matrix_UB_12      -0.0862069000
_diffrn_orient_matrix_UB_13      -0.0152984000
_diffrn_orient_matrix_UB_21      0.0545635000
_diffrn_orient_matrix_UB_22      -0.0405944000
_diffrn_orient_matrix_UB_23      0.0664597000
_diffrn_orient_matrix_UB_31      -0.0766698000
_diffrn_orient_matrix_UB_32      0.0243127000
_diffrn_orient_matrix_UB_33      0.0567656000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10975
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.005
_diffrn_reflns_theta_max         67.005
_diffrn_reflns_theta_min         4.858
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.020
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39050
_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 light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3554
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0521
_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^)+(0.1066P)^2^+1.9795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3119
_reflns_number_total             3554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2019-276-1.CIF
_cod_data_source_block           2
_cod_original_cell_volume        3978.40(13)
_cod_database_code               1563786
_shelx_estimated_absorpt_t_max   0.146
_shelx_estimated_absorpt_t_min   0.098
_reflns_odcompleteness_completeness 99.85
_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 C(H,H,H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C10-C11'
 1.5 with sigma of 0.01
3. Others
 Sof(H10C)=Sof(H10D)=Sof(C11')=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(1)
4.a Free rotating group:
 OW2(HW2A,HW2B)
4.b Rotating group:
 OW1(HW1A,HW1B)
4.c Ternary CH refined with riding coordinates:
 N2(H2)
4.d Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C10(H10C,
 H10D)
4.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C11'(H11D,H11E,H11F), N1(H1A,H1B,H1C)
;