Fluorescent carbon dot‒molecular salt hydrogels
Cayuela, Angelina; Kennedy, Stuart R.; Soriano, M. Laura; Jones, Christopher D.; Valcárcel, Miguel; Steed, Jonathan W.; Chem. Sci. 6 (2015) 6139–; doi:10.1039/C5SC01859E

data_1529299
_publ_section_title
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 Fluorescent carbon dot--molecular salt hydrogels
;
_journal_issue                   11
_journal_name_full               'Chem. Sci.'
_journal_page_first              6139
_journal_paper_doi               10.1039/C5SC01859E
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C28 H28 N4 O8, 2(C6 H16 N), C3 H7 O'
_chemical_formula_sum            'C43 H68 N6 O9'
_chemical_formula_weight         813.03
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-22 deposited with the CCDC.
2015-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.128(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3147(6)
_cell_length_b                   19.2037(13)
_cell_length_c                   14.1567(10)
_cell_measurement_reflns_used    9691
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22.95
_cell_measurement_theta_min      2.51
_cell_volume                     2210.0(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.15
_diffrn_measured_fraction_theta_full 0.768
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_laue_measured_fraction_full 0.768
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18991
_diffrn_reflns_point_group_measured_fraction_full 0.761
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.985
_diffrn_reflns_theta_min         2.121
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.7321
_exptl_absorpt_correction_T_min  0.5259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1379 before and 0.1163 after correction.
The Ratio of minimum to maximum transmission is 0.7183.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       Block
_exptl_crystal_F_000             880
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: propan-1-ol'
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 2190 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.1(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         6058
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0890P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1492
_reflns_Friedel_coverage         0.919
_reflns_friedel_fraction_full    0.753
_reflns_friedel_fraction_max     0.981
_reflns_number_gt                5189
_reflns_number_total             6058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc01859e2.cif
_cod_data_source_block           a028a12
_cod_depositor_comments          'Adding full bibliography for 1529299.cif.'
_cod_database_code               1529299
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.979
_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 O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C41-C42
 1.54 with sigma of 0.02
 C42-C43
 1.54 with sigma of 0.02
 C46-C45
 1.54 with sigma of 0.02
 C45-C44
 1.54 with sigma of 0.02
 C49-C48
 1.54 with sigma of 0.02
 C48-C47
 1.54 with sigma of 0.02
3. Others
 Fixed Sof: C41(0.5) H41A(0.5) H41B(0.5) C42(0.5) H42A(0.5) H42B(0.5) C43(0.5)
 H43A(0.5) H43B(0.5) H43C(0.5) C44(0.3) H44A(0.3) H44B(0.3) C45(0.3) H45A(0.3)
 H45B(0.3) C46(0.3) H46A(0.3) H46B(0.3) H46C(0.3) C47(0.2) H47A(0.2) H47B(0.2)
 C48(0.2) H48A(0.2) H48B(0.2) C49(0.2) H49A(0.2) H49B(0.2) H49C(0.2)
4.a Ternary CH refined with riding coordinates:
 N5(H5A), N6(H6A)
4.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B), C37(H37A,
 H37B), C39(H39A,H39B), C41(H41A,H41B), C42(H42A,H42B), C44(H44A,H44B),
 C45(H45A,H45B), C47(H47A,H47B), C48(H48A,H48B)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1A), N2(H2), N3(H3), N4(H4), C4(H4A), C5(H5), C7(H7), C13(H13), C14(H14),
 C15(H15), C17(H17), C23(H23), C24(H24), C27(H27)
4.d Tetrahedral OH refined with riding coordinates:
 O1(H1), O6(H6)
4.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,
 H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C43(H43A,H43B,H43C),
 C46(H46A,H46B,H46C), C49(H49A,H49B,H49C)
;
_olex2_submission_special_instructions 'No special instructions were received'