From fluorogen to fluorophore by elucidation and suppression of ultrafast excited state processes of a Schiff base
Dasgupta, Souradip; Banerjee, Shrobona; Das, Sharmistha; Datta, Anindya; Physical Chemistry Chemical Physics  (2021) –; doi:10.1039/D1CP02540F

data_7243365
_publ_section_title
;
 From fluorogen to fluorophore by elucidation and suppression of ultrafast
 excited state processes of a Schiff base
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D1CP02540F
_journal_year                    2021
_chemical_formula_moiety         'C30 H28 N4 O6 Zn2'
_chemical_formula_sum            'C30 H28 N4 O6 Zn2'
_chemical_formula_weight         671.30
_chemical_name_systematic        ZnSALAMPY
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-11
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-07-30 deposited with the CCDC.	2021-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.970(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   23.5031(7)
_cell_length_b                   14.9393(4)
_cell_length_c                   33.0899(10)
_cell_measurement_reflns_used    8989
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.8420
_cell_measurement_theta_min      2.5010
_cell_volume                     11112.6(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      150
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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   -110.00  44.00   0.50    8.00    --  -20.00   0.00-108.00  308
  2  \w    -71.00 -28.50   0.50    8.00    --  -20.00 -72.00-180.00   85
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0115718000
_diffrn_orient_matrix_UB_12      -0.0439960000
_diffrn_orient_matrix_UB_13      -0.0041193000
_diffrn_orient_matrix_UB_21      0.0110033000
_diffrn_orient_matrix_UB_22      -0.0027227000
_diffrn_orient_matrix_UB_23      -0.0177618000
_diffrn_orient_matrix_UB_31      0.0272136000
_diffrn_orient_matrix_UB_32      -0.0176771000
_diffrn_orient_matrix_UB_33      0.0130278000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            20252
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.507
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.779
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.605
_exptl_crystal_description       block
_exptl_crystal_F_000             5504
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.091
_refine_diff_density_max         1.283
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.118
_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     761
_refine_ls_number_reflns         9490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0796P)^2^+1.3177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5671
_reflns_number_total             9490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp02540f2.cif
_cod_data_source_block           ad-sdg-zn-salampy_mo
_cod_depositor_comments
;

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C60 H56 N8 O12 Zn4'
_cod_original_formula_weight         1342.60
_cod_original_formula_moiety         '2(C30 H28 N4 O6 Zn2)'
_cod_original_formula_units_Z            8
_cod_database_code               7243365
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C50N4H50O4Zn1
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.717
_reflns_odcompleteness_completeness 83.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.12
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C37(H37A,H37B), C8(H8A,H8B), C50(H50A,H50B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C31(H31), C16(H16), C33(H33), C7(H7), C15(H15), C20(H20), C39(H39),
 C32(H32), C45(H45), C4(H4), C36(H36), C2(H2), C44(H44), C17(H17), C52(H52),
 C54(H54), C46(H46), C23(H23), C49(H49), C40(H40), C24(H24), C34(H34), C53(H53),
  C26(H26), C42(H42), C55(H55), C41(H41), C47(H47), C25(H25), C18(H18),
 C10(H10), C5(H5), C13(H13), C11(H11), C12(H12)
2.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C59(H59A,H59B,H59C), C56(H56A,H56B,
 H56C)
;
_shelx_res_checksum              64147
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.261
_oxdiff_exptl_absorpt_empirical_full_min 0.783