N-methylimidazolium containing metal phosphate-oxalates: solvent-free synthesis, crystal structure, and proton conduction
Zhang, Junfeng; Lei, Qing; Luan, Lindong; Zeng, Hongmei; Zou, Guohong; Lin, Zhien; CrystEngComm  (2022) –; doi:10.1039/D1CE01659H

data_7244121
_publ_section_title
;
 N-methylimidazolium containing metal phosphate-oxalates: solvent-free
 synthesis, crystal structure, and proton conduction
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01659H
_journal_year                    2022
_chemical_formula_moiety         'C7 H6 In N O8 P'
_chemical_formula_sum            'C7 H6 In N O8 P'
_chemical_formula_weight         377.92
_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     dual
_audit_block_doi                 10.5517/ccdc.csd.cc288d32
_audit_creation_date             2021-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-30 deposited with the CCDC.	2022-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                114.317(7)
_cell_angle_beta                 95.498(6)
_cell_angle_gamma                105.293(7)
_cell_formula_units_Z            2
_cell_length_a                   6.6218(4)
_cell_length_b                   9.3168(8)
_cell_length_c                   9.4721(7)
_cell_measurement_reflns_used    3024
_cell_measurement_temperature    290.77(11)
_cell_measurement_theta_max      71.3860
_cell_measurement_theta_min      5.2450
_cell_volume                     499.59(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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      290.77(11)
_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
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -54.00  33.00   1.00    1.00    --  -35.23  57.00 120.00   87
  2  \w    -64.00  34.00   1.00    1.00    --  -35.23  77.00-120.00   98
  3  \w     13.00 106.00   1.00    1.00    --   35.23  38.00-150.00   93
  4  \w     17.00 104.00   1.00    1.00    --   35.23  57.00 -30.00   87
  5  \w     17.00 104.00   1.00    1.00    --   35.23  57.00  30.00   87
  6  \w     17.00 104.00   1.00    1.00    --   35.23  57.00   0.00   87
  7  \w     17.00 104.00   1.00    1.00    --   35.23  57.00 -60.00   87
  8  \w     23.00  90.00   1.00    1.00    --   35.23-125.00 120.00   67
  9  \w     87.00 177.00   1.00    1.00    --  106.90  45.00   0.00   90
 10  \w     37.00 110.00   1.00    1.00    --  106.90 -94.00 -90.00   73
 11  \w    100.00 178.00   1.00    1.00    --  106.90 111.00-180.00   78
 12  \w     39.00 127.00   1.00    1.00    --  106.90 -61.00 -90.00   88
 13  \w     36.00 113.00   1.00    1.00    --  106.90-111.00  30.00   77
 14  \w     36.00 113.00   1.00    1.00    --  106.90-111.00-180.00   77
 15  \w     87.00 177.00   1.00    1.00    --  106.90  45.00-120.00   90
 16  \w     39.00 127.00   1.00    1.00    --  106.90 -61.00  30.00   88
 17  \w    100.00 178.00   1.00    1.00    --  106.90 111.00  60.00   78
 18  \w     37.00 110.00   1.00    1.00    --  106.90 -94.00-120.00   73
 19  \w     36.00 113.00   1.00    1.00    --  106.90-111.00  90.00   77
 20  \w     87.00 175.00   1.00    1.00    --  106.90  61.00 -90.00   88
 21  \w     87.00 177.00   1.00    1.00    --  106.90  45.00-180.00   90
 22  \w     39.00 127.00   1.00    1.00    --  106.90 -61.00 150.00   88
 23  \w     81.00 178.00   1.00    1.00    --  106.90  30.00 120.00   97
 24  \w    -57.00  35.00   1.00    1.00    --  -35.23  38.00-150.00   92
 25  \w      7.00 104.00   1.00    1.00    --   35.23  77.00-150.00   97
 26  \w    -33.00  54.00   1.00    1.00    --   35.23 -57.00 -90.00   87
 27  \w    -33.00  54.00   1.00    1.00    --   35.23 -57.00 -30.00   87
 28  \w      7.00 104.00   1.00    1.00    --   35.23  77.00  30.00   97
 29  \w     17.00 104.00   1.00    1.00    --   35.23  57.00 120.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0847181000
_diffrn_orient_matrix_UB_12      0.1187139000
_diffrn_orient_matrix_UB_13      -0.0439676000
_diffrn_orient_matrix_UB_21      0.1860427000
_diffrn_orient_matrix_UB_22      0.1508631000
_diffrn_orient_matrix_UB_23      0.1293295000
_diffrn_orient_matrix_UB_31      0.1403902000
_diffrn_orient_matrix_UB_32      -0.0146083000
_diffrn_orient_matrix_UB_33      -0.1225365000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0561
_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       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5120
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.050
_diffrn_reflns_theta_max         67.050
_diffrn_reflns_theta_min         5.269
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.864
_exptl_absorpt_correction_T_max  0.189
_exptl_absorpt_correction_T_min  0.015
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.512
_exptl_crystal_description       block
_exptl_crystal_F_000             366
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.206
_refine_diff_density_max         1.363
_refine_diff_density_min         -1.671
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0923P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1713
_reflns_number_total             1781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01659h2.cif
_cod_data_source_block           1
_cod_original_cell_volume        499.59(7)
_cod_database_code               7244121
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C14  H12  In2  N2  O16  P2  '
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), C5(H5), C6(H6)
2.b Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              98955
_shelx_hkl_checksum              76258
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.058
_oxdiff_exptl_absorpt_empirical_full_min 0.673