Tunable room temperature phosphorescence and energy transfer in ratiometric co-crystals.
Zhou, Bo; Zhao, Qihang; Tang, Longchang; Yan, Dongpeng; Chemical communications (Cambridge, England) 56 (2020) 7698–7701; doi:10.1039/d0cc02730h

data_7126707
_publ_section_title
;
 Tunable room temperature phosphorescence and energy transfer in
 ratiometric co-crystals.
;
_journal_issue                   56
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7698
_journal_page_last               7701
_journal_paper_doi               10.1039/d0cc02730h
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C9 H5 O6, C3 H7 N6, 2(H2 O)'
_chemical_formula_sum            'C12 H16 N6 O8'
_chemical_formula_weight         372.31
_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
_audit_creation_date             2018-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-18 deposited with the CCDC.	2020-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                63.563(14)
_cell_angle_beta                 71.551(13)
_cell_angle_gamma                73.220(12)
_cell_formula_units_Z            2
_cell_length_a                   9.3092(13)
_cell_length_b                   9.8441(14)
_cell_length_c                   10.1956(14)
_cell_measurement_reflns_used    1244
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.0950
_cell_measurement_theta_min      4.0400
_cell_volume                     781.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.974
_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    -81.00  20.00   1.00    8.00    --  -11.20 -77.00   0.00  101
  2  \w    -61.00  37.00   1.00    8.00    --   12.45 -57.00 120.00   98
  3  \w    -14.00  79.00   1.00    8.00    --   12.45  57.00 -90.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0478403000
_diffrn_orient_matrix_UB_12      -0.0521335000
_diffrn_orient_matrix_UB_13      0.0572426000
_diffrn_orient_matrix_UB_21      0.0449820000
_diffrn_orient_matrix_UB_22      -0.0596344000
_diffrn_orient_matrix_UB_23      -0.0242800000
_diffrn_orient_matrix_UB_31      0.0483824000
_diffrn_orient_matrix_UB_32      -0.0200779000
_diffrn_orient_matrix_UB_33      0.0497476000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5343
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.593
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
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    1.582
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3115
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0660
_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^)+(0.0572P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1942
_reflns_number_total             3115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02730h2.cif
_cod_data_source_block           20180615a
_cod_depositor_comments
'Adding full bibliography for 7126707--7126708.cif.'
_cod_database_code               7126707
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C1H1N1O1
_chemical_oxdiff_usercomment     ZB-5201
_reflns_odcompleteness_completeness 99.75
_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, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.02
 O8-H8B
 0.9 with sigma of 0.02
3.a Free rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3B), C3(H3A), C6(H6), C5(H5A)
3.c X=CH2 refined with riding coordinates:
 N6(H6A,H6B), N5(H5B,H5C), N4(H4A,H4B)
3.d Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              23622
_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 1.391
_oxdiff_exptl_absorpt_empirical_full_min 0.756