A dual-function metal phosphate for high proton conduction and selective luminescence turn-on sensing of Co2+ ions
Zhou, Shufang; wu, guomei; Lin, Tian; Zhang, Chenxi; Wang, Qing-Lun; CrystEngComm  (2020) –; doi:10.1039/C9CE02031D

data_7239836
_publ_section_title
;
 A dual-function metal phosphate for high proton conduction and selective
 luminescence turn-on sensing of Co2+ ions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE02031D
_journal_year                    2020
_chemical_formula_moiety         'C6 H14 N2 O6 P2 Zn, H2 O'
_chemical_formula_sum            'C6 H16 N2 O7 P2 Zn'
_chemical_formula_weight         355.52
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-22 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                64.183(3)
_cell_angle_beta                 86.148(2)
_cell_angle_gamma                78.931(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3178(2)
_cell_length_b                   8.9144(2)
_cell_length_c                   8.9870(3)
_cell_measurement_reflns_used    3818
_cell_measurement_temperature    299.6(3)
_cell_measurement_theta_max      74.6420
_cell_measurement_theta_min      5.4360
_cell_volume                     588.60(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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      299.6(3)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.955
_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    -11.00  88.00   0.50    0.57    --    0.00  57.00 120.00  198
  2  \w    -22.00  41.00   0.50    0.57    --    0.00  57.00   0.00  126
  3  \w    -23.00  29.00   0.50    0.57    --    0.00 -38.00 120.00  104
  4  \w    -89.00 -60.00   0.50    0.57    --    0.00 -38.00 120.00   58
  5  \w     79.00 106.00   0.50    2.29    --   97.10 -82.00   0.00   54
  6  \w     12.00 117.00   0.50    2.29    --   97.10 -61.00 -90.00  210
  7  \w      9.00 133.00   0.50    2.29    --   97.10 -82.00 -90.00  248
  8  \w     65.00 131.00   0.50    2.29    --   97.10 -30.00 -30.00  132
  9  \w     97.00 128.00   0.50    2.29    --   97.10 -30.00  90.00   62
 10  \w      9.00  46.00   0.50    2.29    --   97.10 -30.00 -30.00   74
 11  \w     78.00 127.00   0.50    2.29    --   97.10 -82.00 120.00   98
 12  \w     10.00  93.00   0.50    2.29    --   97.10 -30.00  90.00  166
 13  \w    149.00 186.00   0.50    2.29    --   97.10   0.00 -60.00   74
 14  \w      9.00  93.00   0.50    2.29    --   97.10 -61.00  60.00  168
 15  \w     81.00 106.00   0.50    2.29    --   97.10 -82.00-180.00   50
 16  \w    126.00 167.00   0.50    2.29    --   97.10  61.00 -60.00   82
 17  \w      9.00  47.00   0.50    2.29    --   97.10 -82.00  60.00   76
 18  \w     63.00 122.00   0.50    2.29    --   97.10 -82.00  60.00  118
 19  \w     11.00 141.00   0.50    2.29    --   97.10   0.00 -60.00  260
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0408250000
_diffrn_orient_matrix_UB_12      0.1743350000
_diffrn_orient_matrix_UB_13      -0.1179072000
_diffrn_orient_matrix_UB_21      0.1435195000
_diffrn_orient_matrix_UB_22      -0.0871148000
_diffrn_orient_matrix_UB_23      -0.0687863000
_diffrn_orient_matrix_UB_31      -0.1156031000
_diffrn_orient_matrix_UB_32      0.0111639000
_diffrn_orient_matrix_UB_33      -0.1328199000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5341
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.895
_diffrn_reflns_theta_min         5.420
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.802
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.006
_exptl_crystal_description       block
_exptl_crystal_F_000             364
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0419P)^2^+0.5264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2146
_reflns_number_total             2303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce02031d2.cif
_cod_data_source_block           2
_cod_database_code               7239836
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     7016
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O7(H7A,H7B)
2.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
2.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C5(H5A,H5B), C2(H2A,H2B), C6(H6A,H6B), C3(H3A,H3B)
;
_shelx_res_checksum              48771
_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 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.894