Sensing of tryptophan by a non-toxic Cobalt(II) complex
DALAI, SUDIPTA; Jana, Swapan Kumar; Mandal, Amit; Kumar, Anoop; Puschmann, Horst; Hossain, Maidul; RSC Adv.  (2016) –; doi:10.1039/C6RA16086G

data_7226704
_publ_section_title
;
 Sensing of tryptophan by a non-toxic Cobalt(II) complex
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA16086G
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C56 H56 Co N8 O8, 2(Cl O4)'
_chemical_formula_sum            'C56 H56 Cl2 Co N8 O16'
_chemical_formula_weight         1226.91
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-08-21
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.06.29 svn.r3191 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2015-08-21 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8148(3)
_cell_length_b                   11.8148(3)
_cell_length_c                   20.5068(8)
_cell_measurement_reflns_used    4536
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.0650
_cell_measurement_theta_min      1.9860
_cell_volume                     2862.53(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1511
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -95.00  -35.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1383 -178.0000 -150.0000 60

  2 omega  -93.00   17.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1383  -19.0000   60.0000 110

  3 omega    3.00   84.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       21.7633   57.0000  -90.0000 81

  4 omega  -47.00   50.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       21.7633  -77.0000  150.0000 97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0381755000
_diffrn_orient_matrix_UB_12      0.0050715000
_diffrn_orient_matrix_UB_13      -0.0265249000
_diffrn_orient_matrix_UB_21      -0.0018002000
_diffrn_orient_matrix_UB_22      0.0594922000
_diffrn_orient_matrix_UB_23      0.0046285000
_diffrn_orient_matrix_UB_31      0.0462836000
_diffrn_orient_matrix_UB_32      0.0064829000
_diffrn_orient_matrix_UB_33      -0.0216995000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18765
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.492
_diffrn_reflns_theta_min         1.986
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           35
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1274
_exptl_crystal_recrystallization_method
'The material was recrystallised from water by slow evaporation'
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.1213
_exptl_crystal_size_min          0.0955
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 987 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0329P)^2^+0.9214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2638
_reflns_number_total             2960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra16086g2.cif
_cod_data_source_block           ind_9684
_cod_original_cell_volume        2862.55(18)
_cod_database_code               7226704
_chemical_oxdiff_formula         C56H56Cl2CoN8O16
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C8(H8), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              10355
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2014-03-21
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a hair in perfluoroether oil'
_olex2_submission_special_instructions 'No special instructions were received'