Schiff base triggering synthesis of copper(II) complex and its catalytic fate towards mimics of phenoxazinone synthase activity
Kumar Mudi, Prafullya; Bandopadhyay, Nilaj; Joshi, Mayank; Shit, Madhusudan; Paul, Suvendu; Roy Choudhury, Angshuman; Biswas, Bhaskar; Inorganica Chimica Acta 505 (2020) 119468–; doi:10.1016/j.ica.2020.119468

data_1565211
_publ_section_title
;
 Schiff base triggering synthesis of copper(II) complex and its catalytic
 fate towards mimics of phenoxazinone synthase activity
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119468
_journal_paper_doi               10.1016/j.ica.2020.119468
_journal_volume                  505
_journal_year                    2020
_chemical_formula_moiety         'C45 H42 Cu2 N3 O9, Cl O4'
_chemical_formula_sum            'C45 H42 Cl Cu2 N3 O13'
_chemical_formula_weight         995.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.6993(10)
_cell_length_b                   15.1138(9)
_cell_length_c                   26.913(2)
_cell_measurement_reflns_used    5029
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      31.9480
_cell_measurement_theta_min      2.7920
_cell_volume                     8419.6(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -69.00 118.20   0.30   15.00    --   29.89  54.00 -60.00  624
  2  \w     12.00 118.20   0.30   15.00    --   29.89  54.00 -60.00  354
  3  \w      3.00  29.10   0.30   15.00    --   29.89  54.00-150.00   87
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0028670000
_diffrn_orient_matrix_UB_12      -0.0237849000
_diffrn_orient_matrix_UB_13      -0.0226022000
_diffrn_orient_matrix_UB_21      -0.0060848000
_diffrn_orient_matrix_UB_22      0.0393624000
_diffrn_orient_matrix_UB_23      -0.0135405000
_diffrn_orient_matrix_UB_31      0.0336149000
_diffrn_orient_matrix_UB_32      0.0092678000
_diffrn_orient_matrix_UB_33      -0.0005611000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40939
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.502
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       plate
_exptl_crystal_F_000             4096
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.191
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         7402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0685
_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^)+(0.1260P)^2^+18.6138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.2393
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4802
_reflns_number_total             7402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-505-119468.cif
_cod_data_source_block           p11_cu_100k
_cod_original_cell_volume        8419.5(9)
_cod_database_code               1565211
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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:
 C00L(H00L), C00O(H00O), C00Q(H00Q), C00U(H00U), C010(H010), C011(H011),
 C012(H012), C014(H014), C015(H015), C017(H017), C018(H018), C019(H019),
 C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D), C01E(H01E), C01G(H01I),
 C01H(H01J), C01I(H01K), C01J(H01L), C01O(H01V), C01P(H01W), C01Q(H01X)
2.b Idealised Me refined as rotating group:
 C01F(H01F,H01G,H01H), C01K(H01M,H01N,H01O), C01L(H01P,H01Q,H01R), C01M(H01S,
 H01T,H01U), C01R(H01Y,H,HA), C01S(H01Z,HB,HC)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.646
_oxdiff_exptl_absorpt_empirical_full_min 0.525