Cubane-like tetranuclear Cu(ii) complexes bearing a Cu4O4 core: crystal structure, magnetic properties, DFT calculations and phenoxazinone synthase like activity.
Sagar, Shipra; Sengupta, Swaraj; Mota, Antonio J.; Chattopadhyay, Shyamal K.; Espinosa Ferao, Arturo; Riviere, Eric; Lewis, William; Naskar, Subhendu; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1249–1259; doi:10.1039/c6dt03754b

data_7041513
_publ_section_title
;
 Cubane-like tetranuclear Cu(ii) complexes bearing a Cu4O4 core: crystal
 structure, magnetic properties, DFT calculations and phenoxazinone
 synthase like activity.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1249
_journal_page_last               1259
_journal_paper_doi               10.1039/c6dt03754b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C10 H7 Cl N2 O S'
_chemical_formula_sum            'C10 H7 Cl N2 O S'
_chemical_formula_weight         238.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-09-27 deposited with the CCDC.
2016-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.866(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7035(4)
_cell_length_b                   3.79321(9)
_cell_length_c                   17.8136(5)
_cell_measurement_reflns_used    2257
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.8210
_cell_measurement_theta_min      4.9590
_cell_volume                     992.28(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
  1 omega  -50.00   33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -180.0000 83

  2 omega -124.00   47.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000    0.0000    0.0000 171

  3 omega   33.00  135.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000 -180.0000 102

  4 omega   31.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000    0.0000 59

  5 omega   35.00   98.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -120.0000 63

  6 omega   35.00   98.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  -30.0000 63

  7 omega   82.00  174.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000  -30.0000 92

  8 omega   82.00  174.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000 -150.0000 92

  9 omega   36.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000  150.0000 73
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      0.0938315000
_diffrn_orient_matrix_UB_12      -0.1519192000
_diffrn_orient_matrix_UB_13      0.0249436000
_diffrn_orient_matrix_UB_21      -0.0441136000
_diffrn_orient_matrix_UB_22      -0.2120328000
_diffrn_orient_matrix_UB_23      0.0623228000
_diffrn_orient_matrix_UB_31      -0.0157193000
_diffrn_orient_matrix_UB_32      -0.3115991000
_diffrn_orient_matrix_UB_33      -0.0546658000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4575
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.048
_diffrn_reflns_theta_min         4.972
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    5.145
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       needle
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.3147
_exptl_crystal_size_mid          0.0747
_exptl_crystal_size_min          0.0481
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0757P)^2^+0.4323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1768
_reflns_number_total             1965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03754b2.cif
_cod_data_source_block           snwllj
_cod_depositor_comments
'Adding full bibliography for 7041513--7041515.cif.'
_cod_database_code               7041513
_nottingham_internal_coll_name   SNWLLJ
_nottingham_internal_coll_number 14537
_nottingham_internal_coll_client SN/WL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '2.0000, 8.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pczwl
_nottingham_internal_coll_date   30/03/2015
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 27/05/2015
_nottingham_internal_process_user pczwl
_nottingham_internal_solution_date 27/5/2015
_nottingham_internal_solution_user pczwl
_nottingham_internal_refinement_date 3/6/2015
_nottingham_internal_refinement_user pczwl
_nottingham_internal_validation_date 3/6/2015
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 3/6/2015
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C10 H7 N2 O Cl S'
_chemical_oxdiff_usercomment
'SNWLLJ #14537 GVB-479 on micromount in fomblin film FOR SN/WL'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C13(H13)
;
_shelx_res_checksum              95903
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'