New group IIIA metal phosphate-oxalates containing dimethylammonium cations with proton conductivity.
Pan, Tian-Yu; Wen, Wei-Yang; Ma, Wen; Zheng, Shou-Tian; Feng, Mei-Ling; Huang, Xiao-Ying; Dalton transactions (Cambridge, England : 2003) 53 (2024) 2318–2323; doi:10.1039/d3dt03368f

data_7714973
_publ_section_title
;
 New group IIIA metal phosphate-oxalates containing dimethylammonium
 cations with proton conductivity.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2318
_journal_page_last               2323
_journal_paper_doi               10.1039/d3dt03368f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C2 H6 In2 O20 P4, 2(C2 H8 N), H2 O'
_chemical_formula_sum            'C6 H24 In2 N2 O21 P4'
_chemical_formula_weight         813.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-09-26
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-29 deposited with the CCDC.	2023-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.95360(10)
_cell_length_b                   10.26900(10)
_cell_length_c                   13.16290(10)
_cell_measurement_reflns_used    8951
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      74.7310
_cell_measurement_theta_min      3.3560
_cell_volume                     1204.60(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11935
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.170
_diffrn_reflns_theta_min         3.373
_exptl_absorpt_coefficient_mu    18.729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    2.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.179
_refine_diff_density_min         -1.638
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.000(8)
_refine_ls_extinction_coef       0.00041(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4430
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0548P)^2^+0.1034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0791
_reflns_Friedel_coverage         0.738
_reflns_Friedel_fraction_full    0.869
_reflns_Friedel_fraction_max     0.807
_reflns_number_gt                4368
_reflns_number_total             4430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03368f2.cif
_cod_data_source_block           x_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7714971--7714973.cif.'
_cod_database_code               7714973
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.603
_shelx_estimated_absorpt_t_min   0.316
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9997
 0.0003
2. Restrained distances
 O21-H21A = O21-H21B
 0.82 with sigma of 0.01
 O14-H14 = O11-H11
 0.82 with sigma of 0.01
 H21B-H2A
 2.1 with sigma of 0.01
 H21A-H21B
 1.39 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
3.b Tetrahedral OH refined with riding coordinates:
 O2(H2C), O3(H3D), O7(H7A), O8(H8A)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              43134
_olex2_submission_special_instructions 'No special instructions were received'