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_7244122
_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         'C H3 Fe O10 P2, C4 H7 N2'
_chemical_formula_sum            'C5 H10 Fe N2 O10 P2'
_chemical_formula_weight         375.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-13 deposited with the CCDC.	2022-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.467(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1586(2)
_cell_length_b                   10.0083(3)
_cell_length_c                   12.7498(4)
_cell_measurement_reflns_used    2678
_cell_measurement_temperature    295.7(5)
_cell_measurement_theta_max      71.2290
_cell_measurement_theta_min      4.8130
_cell_volume                     1165.12(6)
_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      295.7(5)
_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    -53.00  33.00   1.00    1.76    --  -34.98  57.00-120.00   86
  2  \w   -106.00  36.00   1.00    1.76    --  -34.98   0.00-150.00  142
  3  \w      1.00  75.00   1.00    1.76    --   34.98 -99.00 150.00   74
  4  \w     23.00  90.00   1.00    1.76    --   34.98-125.00 -60.00   67
  5  \w     16.00 103.00   1.00    1.76    --   34.98  57.00-150.00   87
  6  \w     23.00  90.00   1.00    1.76    --   34.98-125.00 150.00   67
  7  \w     87.00 177.00   1.00    7.04    --  106.90  45.00-180.00   90
  8  \w     87.00 175.00   1.00    7.04    --  106.90  61.00 -90.00   88
  9  \w     35.00 133.00   1.00    7.04    --  106.90 -30.00 -90.00   98
 10  \w     37.00 110.00   1.00    7.04    --  106.90 -94.00 -60.00   73
 11  \w     35.00 133.00   1.00    7.04    --  106.90 -30.00   0.00   98
 12  \w    100.00 178.00   1.00    7.04    --  106.90 111.00  90.00   78
 13  \w     38.00 136.00   1.00    7.04    --  106.90 -77.00   0.00   98
 14  \w   -103.00 -16.00   1.00    1.76    --  -34.98 -57.00  90.00   87
 15  \w      6.00  86.00   1.00    1.76    --   34.98  77.00   0.00   80
 16  \w    -36.00  57.00   1.00    1.76    --   34.98 -38.00 -60.00   93
;
_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      0.0081388000
_diffrn_orient_matrix_UB_12      -0.0283248000
_diffrn_orient_matrix_UB_13      0.1190567000
_diffrn_orient_matrix_UB_21      -0.1635707000
_diffrn_orient_matrix_UB_22      0.0348484000
_diffrn_orient_matrix_UB_23      0.0018370000
_diffrn_orient_matrix_UB_31      -0.0405376000
_diffrn_orient_matrix_UB_32      -0.1472199000
_diffrn_orient_matrix_UB_33      -0.0226736000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6287
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.041
_diffrn_reflns_theta_max         67.041
_diffrn_reflns_theta_min         4.843
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.596
_exptl_absorpt_correction_T_max  0.215
_exptl_absorpt_correction_T_min  0.020
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.83
_exptl_crystal_size_mid          0.313
_exptl_crystal_size_min          0.271
_refine_diff_density_max         1.042
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1154P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1911
_reflns_number_total             2071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01659h2.cif
_cod_data_source_block           2
_cod_database_code               7244122
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C20  H40  Fe4  N8  O40  P8  '
_shelx_estimated_absorpt_t_max   0.120
_shelx_estimated_absorpt_t_min   0.031
_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 C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3A), C4(H4), C5(H5)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
2.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O7(H7), O8(H8)
;
_shelx_res_checksum              80056