Two histidine-templated metal phosphate-oxalates: solvent-free synthesis, luminescence, and proton-conducting properties.
Li, Ying; Wang, Yulin; Cheng, Juan; Huang, Ling; Gao, Daojiang; Zou, Guohong; Zhao, Yan; Lin, Zhien; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9675–9679; doi:10.1039/d4dt01217h

data_7716190
_publ_section_title
;
 Two histidine-templated metal phosphate-oxalates: solvent-free synthesis,
 luminescence, and proton-conducting properties.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9675
_journal_page_last               9679
_journal_paper_doi               10.1039/d4dt01217h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C16 H22 In2 N6 O20 P2'
_chemical_formula_sum            'C16 H22 In2 N6 O20 P2'
_chemical_formula_weight         909.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-04-22 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.8422(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.40930(12)
_cell_length_b                   10.12355(16)
_cell_length_c                   30.4576(3)
_cell_measurement_reflns_used    5637
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.1150
_cell_measurement_theta_min      5.2200
_cell_volume                     2591.58(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_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
;
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    3.10    --  -35.23  57.00 -90.00   87
  2  \w    -57.00  35.00   1.00    3.10    --  -35.23  38.00  30.00   92
  3  \w   -109.00 -35.00   1.00    3.10    --  -35.23-178.00 120.00   74
  4  \w    -37.00  73.00   1.00    3.10    --   35.23 -19.00 -90.00  110
  5  \w     57.00 109.00   1.00    3.10    --   35.23 178.00-120.00   52
  6  \w     57.00 109.00   1.00    3.10    --   35.23 178.00 -90.00   52
  7  \w    -34.00  64.00   1.00    3.10    --   35.23 -77.00  90.00   98
  8  \w     55.00 110.00   1.00    3.10    --   35.23-178.00-150.00   55
  9  \w      1.00  76.00   1.00    3.10    --   35.23 -99.00  30.00   75
 10  \w    100.00 178.00   1.00   12.41    --  107.52 111.00   0.00   78
 11  \w     38.00 136.00   1.00   12.41    --  107.52 -77.00-150.00   98
 12  \w     37.00 109.00   1.00   12.41    --  107.52 -94.00  60.00   72
 13  \w     38.00 136.00   1.00   12.41    --  107.52 -77.00  60.00   98
 14  \w     88.00 153.00   1.00   12.41    --  107.52  61.00 -90.00   65
 15  \w     64.00 106.00   1.00   12.41    --  107.52 -94.00  90.00   42
 16  \w     37.00  81.00   1.00   12.41    --  107.52 -94.00   0.00   44
 17  \w     89.00 123.00   1.00   12.41    --  107.52 -45.00  90.00   34
 18  \w    109.00 172.00   1.00   12.41    --  107.52  61.00-180.00   63
 19  \w     95.00 175.00   1.00   12.41    --  107.52  61.00 120.00   80
;
_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      -0.1682042000
_diffrn_orient_matrix_UB_12      0.0590001000
_diffrn_orient_matrix_UB_13      -0.0060171000
_diffrn_orient_matrix_UB_21      -0.0728563000
_diffrn_orient_matrix_UB_22      -0.1354228000
_diffrn_orient_matrix_UB_23      0.0106727000
_diffrn_orient_matrix_UB_31      0.0014386000
_diffrn_orient_matrix_UB_32      0.0365803000
_diffrn_orient_matrix_UB_33      0.0490962000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14149
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.072
_diffrn_reflns_theta_max         67.072
_diffrn_reflns_theta_min         4.603
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.412
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.436
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         4616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0910P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1532
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3851
_reflns_number_total             4616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01217h2.cif
_cod_data_source_block           lyy2-10-1
_cod_depositor_comments
'Adding full bibliography for 7716190--7716191.cif.'
_cod_database_code               7716190
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.243
_shelx_estimated_absorpt_t_min   0.072
_reflns_odcompleteness_completeness 99.96
_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 C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6A), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C13(H13A,H13B)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N5(H5), N6(H6), C9(H9), C10(H10), C15(H15), C16(H16)
2.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N4(H4A,H4B,H4C)
2.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O8(H8)
;
_shelx_res_checksum              1895
_olex2_date_sample_data_collection 2022-10-10
_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 1.778
_oxdiff_exptl_absorpt_empirical_full_min 0.588