Exploration of an Easily Synthesized Fluorescent Probe for Detecting Copper in Aqueous Samples
Sanmartin Matalobos, Jesus; Garcia-Deibe, Ana M.; Fondo, Matilde; Zarepour-Jevinani, Morteza; Domínguez-González, M. R.; Bermejo-Barrera, Pilar; Dalton Trans.  (2017) –; doi:10.1039/C7DT02872E

data_7044581
_publ_section_title
;
 Exploration of an Easily Synthesized Fluorescent Probe for Detecting
 Copper in Aqueous Samples
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02872E
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C38 H37 Co N6 O5 S2'
_chemical_formula_sum            'C38 H37 Co N6 O5 S2'
_chemical_formula_weight         780.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-04 deposited with the CCDC.
2017-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.525(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3758(9)
_cell_length_b                   10.3171(8)
_cell_length_c                   33.283(3)
_cell_measurement_reflns_used    1082
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.21
_cell_measurement_theta_min      2.33
_cell_volume                     3532.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle)'
_computing_publication_material  'enCIFer 1.6 (CCDC, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -360.00   9.00   0.50   40.00  39.42  14.50  25.50    --   738
  2  \f   -121.60 -29.60   0.50   40.00 -26.96  -8.00  90.50    --   184
  3  \w      3.23  79.23   0.50   40.00    --    4.50  58.00 -25.00  152
;
_diffrn_measurement_device_type  'Bruker AXS X8 kappa APEXII'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0031759000
_diffrn_orient_matrix_UB_12      -0.0664653000
_diffrn_orient_matrix_UB_13      0.0054860000
_diffrn_orient_matrix_UB_21      0.0056088000
_diffrn_orient_matrix_UB_22      0.0174521000
_diffrn_orient_matrix_UB_23      0.0207663000
_diffrn_orient_matrix_UB_31      -0.0686415000
_diffrn_orient_matrix_UB_32      -0.0016562000
_diffrn_orient_matrix_UB_33      -0.0008652000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.0791
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            13764
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.275
_diffrn_reflns_theta_min         1.974
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.68164
_exptl_absorpt_correction_T_min  0.67385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       needle
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.570
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.807
_refine_diff_density_min         -2.055
_refine_diff_density_rms         0.238
_refine_ls_abs_structure_details
;
 Flack x determined using 3541 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     962
_refine_ls_number_reflns         13764
_refine_ls_number_restraints     1591
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1565
_refine_ls_R_factor_gt           0.1245
_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^)+60.7548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2683
_refine_ls_wR_factor_ref         0.2951
_reflns_Friedel_coverage         0.972
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                11883
_reflns_number_total             13764
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9590\% 
around [0.00 -0.00 1.00] (reciprocal) or [0.39 -0.01 0.92] (direct)
;
_cod_data_source_file            c7dt02872e2.cif
_cod_data_source_block           Co(L)(HL)(H2O)
_cod_database_code               7044581
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.705
_shelx_estimated_absorpt_t_max   0.981
_exptl_absorpt_special_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_twin_items               2
_oxdiff_twin_integration_method  simultaneous
_shelx_res_checksum              48946