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_7716191
_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         'C6 H2 Ga2 O20 P2, 2(C6 H11 N3 O2), C2 H2 O4'
_chemical_formula_sum            'C20 H26 Ga2 N6 O28 P2'
_chemical_formula_weight         999.85
_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_creation_date             2023-12-29
_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                89.094(4)
_cell_angle_beta                 89.075(5)
_cell_angle_gamma                87.698(5)
_cell_formula_units_Z            1
_cell_length_a                   7.9866(5)
_cell_length_b                   9.6052(5)
_cell_length_c                   10.7764(6)
_cell_measurement_reflns_used    4867
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.3510
_cell_measurement_theta_min      4.0750
_cell_volume                     825.82(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_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   -107.00  35.00   1.00    1.00    --  -35.73   0.00-150.00  142
  2  \w   -105.00  -7.00   1.00    1.00    --  -35.73 -77.00-120.00   98
  3  \w     55.00 110.00   1.00    1.00    --   35.73-178.00  60.00   55
  4  \w     55.00 110.00   1.00    1.00    --   35.73-178.00-180.00   55
  5  \w     13.00 106.00   1.00    1.00    --   35.73  38.00  30.00   93
  6  \w     55.00 110.00   1.00    1.00    --   35.73-178.00 150.00   55
  7  \w      1.00  76.00   1.00    1.00    --   35.73 -99.00-180.00   75
  8  \w      1.00  76.00   1.00    1.00    --   35.73 -99.00  30.00   75
  9  \w     79.00 177.00   1.00    2.71    --  107.52  77.00   0.00   98
 10  \w     37.00 109.00   1.00    2.71    --  107.52 -94.00-150.00   72
 11  \w     82.00 178.00   1.00    2.71    --  107.52  30.00-180.00   96
 12  \w     37.00 109.00   1.00    2.71    --  107.52 -94.00   0.00   72
 13  \w     36.00 178.00   1.00    2.71    --  107.52   0.00 -30.00  142
 14  \w     38.00 128.00   1.00    2.71    --  107.52 -45.00   0.00   90
 15  \w     57.00 151.00   1.00    2.71    --  107.52 178.00  90.00   94
 16  \w     38.00 128.00   1.00    2.71    --  107.52 -45.00-150.00   90
 17  \w     36.00 112.00   1.00    2.71    --  107.52-111.00 120.00   76
 18  \w     40.00 128.00   1.00    2.71    --  107.52 -61.00  90.00   88
 19  \w     38.00 136.00   1.00    2.71    --  107.52 -77.00 -90.00   98
 20  \w    -58.00  35.00   1.00    1.00    --  -35.73  38.00  30.00   93
 21  \w   -104.00 -17.00   1.00    1.00    --  -35.73 -57.00 120.00   87
 22  \w      7.00 105.00   1.00    1.00    --   35.73  77.00 -30.00   98
 23  \w    -35.00  58.00   1.00    1.00    --   35.73 -38.00-150.00   93
 24  \w      7.00 105.00   1.00    1.00    --   35.73  77.00  60.00   98
 25  \w     57.00 110.00   1.00    1.00    --   35.73 178.00   0.00   53
 26  \w     82.00 178.00   1.00    2.71    --  107.52  30.00  90.00   96
 27  \w     79.00 177.00   1.00    2.71    --  107.52  77.00 -60.00   98
 28  \w     87.00 177.00   1.00    2.71    --  107.52  45.00 120.00   90
;
_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      0.0112332000
_diffrn_orient_matrix_UB_12      0.1584837000
_diffrn_orient_matrix_UB_13      -0.0203787000
_diffrn_orient_matrix_UB_21      -0.0625127000
_diffrn_orient_matrix_UB_22      -0.0140715000
_diffrn_orient_matrix_UB_23      -0.1335418000
_diffrn_orient_matrix_UB_31      -0.1823269000
_diffrn_orient_matrix_UB_32      0.0213768000
_diffrn_orient_matrix_UB_33      0.0468825000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8580
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.073
_diffrn_reflns_theta_max         67.073
_diffrn_reflns_theta_min         4.103
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.057
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52671
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_description       prism
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         2958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0933P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2668
_reflns_number_total             2958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01217h2.cif
_cod_data_source_block           lyy1-141-12a
_cod_depositor_comments
'Adding full bibliography for 7716190--7716191.cif.'
_cod_database_code               7716191
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.396
_reflns_odcompleteness_completeness 99.86
_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:
 C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C8(H8), C9(H9)
2.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
2.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O12(H12), O14(H14)
;
_shelx_res_checksum              23533
_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 2.059
_oxdiff_exptl_absorpt_empirical_full_min 0.687