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_7126708
_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         372.30
_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
;
2018-12-19 deposited with the CCDC.	2020-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                72.186(7)
_cell_angle_beta                 82.829(7)
_cell_angle_gamma                81.819(7)
_cell_formula_units_Z            4
_cell_length_a                   9.4813(8)
_cell_length_b                   11.8746(10)
_cell_length_c                   14.6779(13)
_cell_measurement_reflns_used    2747
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.6040
_cell_measurement_theta_min      3.8550
_cell_volume                     1551.5(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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.986
_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     -9.00  28.00   1.00   10.00    --  -11.20 -99.00-180.00   37
  2  \w    -56.00  36.00   1.00   10.00    --   12.45 -57.00  30.00   92
  3  \w    -11.00  70.00   1.00   10.00    --   12.45  57.00 -30.00   81
  4  \w    -16.00  85.00   1.00   10.00    --   12.45  57.00-180.00  101
;
_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      -0.0340613000
_diffrn_orient_matrix_UB_12      -0.0454008000
_diffrn_orient_matrix_UB_13      0.0356076000
_diffrn_orient_matrix_UB_21      -0.0590828000
_diffrn_orient_matrix_UB_22      0.0112676000
_diffrn_orient_matrix_UB_23      -0.0279995000
_diffrn_orient_matrix_UB_31      0.0332292000
_diffrn_orient_matrix_UB_32      -0.0423863000
_diffrn_orient_matrix_UB_33      -0.0233199000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11545
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         3.472
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82155
_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    1.594
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         6251
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0581P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3803
_reflns_number_total             6251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02730h2.cif
_cod_data_source_block           20180615b
_cod_depositor_comments
;
Adding full bibliography for 7126707--7126708.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C9 H5 O6), 2(C3 H7 N6), 4(H2 O)'
_cod_original_formula_sum        'C24 H32 N12 O16'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     744.61
_cod_database_code               7126708
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C1H1O1N1
_chemical_oxdiff_usercomment     ZB-5202
_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
 O8-H8 = O2-H2
 0.85 with sigma of 0.02
3.a Free rotating group:
 O13(H13A,H13B), O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C12(H12), C13(H13), C15(H15), N5(H5), N12(H12B)
3.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N7(H7A,H7B), N8(H8A,H8B), N9(H9A,H9B)
3.d Idealised tetrahedral OH refined as rotating group:
 O6(H6A), O12(H12A)
;
_shelx_res_checksum              40311
_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 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.798