Isonicotinic acid-templated metal phosphate–oxalates: solvent-free synthesis, luminescence, and proton conduction
Huang, Lijuan; Xu, Haiping; Zhao, Yan; Huang, Ling; Bi, Jian; Zeng, Hongmei; Zou, Guohong; Gao, Daojiang; Lin, Zhien; CrystEngComm 23 (2021) 6855–6858; doi:10.1039/D1CE00873K

data_7243617
_publ_section_title
;
 Isonicotinic acid-templated metal phosphate--oxalates: solvent-free
 synthesis, luminescence, and proton conduction
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              6855
_journal_page_last               6858
_journal_paper_doi               10.1039/D1CE00873K
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C2 H Ga O8 P, C6 H6 N O2, H2 O'
_chemical_formula_sum            'C8 H9 Ga N O11 P'
_chemical_formula_weight         395.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-18
_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.	2021-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.836(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.8667(4)
_cell_length_b                   16.1141(6)
_cell_length_c                   21.1102(14)
_cell_measurement_reflns_used    2203
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9460
_cell_measurement_theta_min      3.4290
_cell_volume                     2675.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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    -25.00  23.00   0.80    5.00    --  -15.32 -99.00 -30.00   60
  2  \w    -52.00  85.60   0.80    5.00    --   17.51   0.00-120.00  172
  3  \w    -50.00  34.00   0.80    5.00    --   17.51 -57.00-120.00  105
  4  \w    -34.00   2.00   0.80    5.00    --  -15.32  38.00 120.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0070197000
_diffrn_orient_matrix_UB_12      0.0063888000
_diffrn_orient_matrix_UB_13      0.0331169000
_diffrn_orient_matrix_UB_21      -0.0464880000
_diffrn_orient_matrix_UB_22      -0.0375237000
_diffrn_orient_matrix_UB_23      0.0025615000
_diffrn_orient_matrix_UB_31      0.0769171000
_diffrn_orient_matrix_UB_32      -0.0220824000
_diffrn_orient_matrix_UB_33      0.0052203000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8197
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.027
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.238
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.965
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         2733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0424P)^2^+5.6814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2335
_reflns_number_total             2733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00873k2.cif
_cod_data_source_block           h3-80-4
_cod_depositor_comments
'Adding full bibliography for 7243616--7243617.cif.'
_cod_database_code               7243617
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c12h12n2o3p1Ga1
_shelx_estimated_absorpt_t_max   0.573
_shelx_estimated_absorpt_t_min   0.517
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H,H) groups
2. Others
 Fixed Sof: O11(0.5) H11A(0.5) H11B(0.5) O12(0.5) H12A(0.5) H12B(0.5)
3.a Free rotating group:
 O11(H11A,H11B), O12(H12A,H12B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C5(H5), C7(H7), C8(H8)
3.c Idealised tetrahedral OH refined as rotating group:
 O4(H4A), O9(H9)
;
_shelx_res_checksum              48562
_shelx_hkl_checksum              97660
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.119
_oxdiff_exptl_absorpt_empirical_full_min 0.917