Rhodamine-azo based two fluorescent probes for recognition of trivalent metal ions: crystal structures elucidation and biological application
Mandal, Jayanta; Pal, Kunal; Ghosh Chowdhury, Sougata; Karmakar, Parimal; Panja, Anangamohan; Banerjee, Snehasis; Saha, Amrita; Dalton Transactions  (2022) –; doi:10.1039/D2DT00399F

data_7711227
_publ_section_title
;
 Rhodamine-azo based two fluorescent probes for recognition of trivalent
 metal ions: crystal structures elucidation and biological application
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00399F
_journal_year                    2022
_chemical_formula_moiety         'C80 H76 Al N13 O7, C3 H7 N O, N O3'
_chemical_formula_sum            'C83 H83 Al N15 O11'
_chemical_formula_weight         1493.62
_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   geom
_audit_creation_date             2022-07-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-06 deposited with the CCDC.	2022-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                92.089(3)
_cell_angle_beta                 106.005(3)
_cell_angle_gamma                90.341(3)
_cell_formula_units_Z            2
_cell_length_a                   13.9132(12)
_cell_length_b                   16.3851(14)
_cell_length_c                   19.9383(17)
_cell_measurement_reflns_used    564
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.90
_cell_volume                     4365.6(7)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1092
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            146421
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.173
_diffrn_reflns_theta_min         1.668
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       block
_exptl_crystal_F_000             1574
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   0.948
_exptl_transmission_factor_min   0.798
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1000
_refine_ls_number_reflns         19276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1618
_refine_ls_R_factor_gt           0.0873
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+3.6704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1971
_refine_ls_wR_factor_ref         0.2378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9909
_reflns_number_total             19276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00399f2.cif
_cod_data_source_block           1
_cod_database_code               7711227
_shelx_shelxl_version_number     2018/3
_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 N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed X: N20(0.1769)
 Fixed Y: N20(0.5436)
 Fixed Z: N20(0.15151)
3.a Secondary CH2 refined with riding coordinates:
 N11(H11A,H11B), C2(H2A,H2B), N14(H14A,H14B), C19(H19A,H19B), C22(H22A,H22B),
 C71(H71A,H71B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C201(H201), C73(H73), C5(H5), C16(H16), N15(H15), C27(H27), C30(H30),
 C33(H33), C34(H34), C35(H35), C36(H36), C40(H40), C44(H44), C45(H45), C46(H46),
  C47(H47), C48(H48), C52(H52), C54(H54), C56(H56), C57(H57), C58(H58),
 C59(H59), C60(H60), C62(H62), C65(H65), C68(H68), C76(H76), C77(H77), C78(H78),
  C79(H79), C80(H80), C81(H81), C84(H84)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C26(H26A,H26B,
 H26C), C32(H32A,H32B,H32C), C42(H42A,H42B,H42C), C51(H51A,H51B,H51C), C61(H61A,
 H61B,H61C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C82(H82A,H82B,H82C),
 C85(H85A,H85B,H85C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              47878
_shelx_hkl_checksum              54237
_shelx_fab_checksum              10422
_olex2_submission_special_instructions 'No special instructions were received'