A reactive oxygen species-generating, cyclooxygenase-2 inhibiting, cancer stem cell-potent tetranuclear copper(II) cluster
Lu, Chunxin; Laws, Kristine; Eskandari, Arvin; Suntharalingam, Kogularamanan; Dalton Trans.  (2017) –; doi:10.1039/C7DT02789C

data_7044098
_publ_section_title
;
 A reactive oxygen species-generating, cyclooxygenase-2 inhibiting, cancer
 stem cell-potent tetranuclear copper(II) cluster
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02789C
_journal_year                    2017
_chemical_formula_moiety
'C76 H66 Cl8 Cu4 N6 O12 S2, 2(C3 H6 N O), 2(C2 H3 N)'
_chemical_formula_sum            'C86 H84 Cl8 Cu4 N10 O14 S2'
_chemical_formula_weight         2083.51
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-12-15
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-05-09 deposited with the CCDC.
2017-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.2803(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.1514(3)
_cell_length_b                   12.63396(19)
_cell_length_c                   21.6626(4)
_cell_measurement_reflns_used    6334
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.1520
_cell_measurement_theta_min      4.1240
_cell_volume                     4645.14(14)
_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
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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, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0802
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.9767
_diffrn_measurement_details
;
  1 omega  -30.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8327  -77.0000  -60.0000 91

  2 omega   25.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8327  -38.0000  120.0000 29

  3 omega    0.00   38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8327  -99.0000   30.0000 38

  4 omega   -3.00   22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8327  -99.0000 -180.0000 25

  5 omega   56.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8327   77.0000   60.0000 47

  6 omega   72.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8327  178.0000 -120.0000 36

  7 omega   56.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8327 -178.0000    0.0000 40

  8 omega   21.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8327   57.0000   60.0000 39

  9 omega   45.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.8327  -99.0000 -180.0000 28

 10 omega   50.00   76.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 26

 11 omega   40.00   81.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 41

 12 omega  121.00  169.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -150.0000 48

 13 omega   41.00   76.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 35

 14 omega   42.00   84.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 42

 15 omega   43.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  120.0000 48

 16 omega   53.00   85.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 32

 17 omega   43.00   86.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -180.0000 43

 18 omega   43.00  108.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -120.0000 65

 19 omega   40.00   97.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   30.0000 57

 20 omega   89.00  171.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -180.0000 82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0463711000
_diffrn_orient_matrix_UB_12      0.1016130000
_diffrn_orient_matrix_UB_13      0.0204145000
_diffrn_orient_matrix_UB_21      0.0738119000
_diffrn_orient_matrix_UB_22      -0.0473404000
_diffrn_orient_matrix_UB_23      -0.0223633000
_diffrn_orient_matrix_UB_31      -0.0252542000
_diffrn_orient_matrix_UB_32      0.0480264000
_diffrn_orient_matrix_UB_33      -0.0651814000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18925
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.349
_diffrn_reflns_theta_min         3.547
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63163
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         8987
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0822P)^2^+0.2334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7095
_reflns_number_total             8987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02789c2.cif
_cod_data_source_block           20161129-2-90
_cod_original_cell_volume        4645.13(13)
_cod_database_code               7044098
_chemical_oxdiff_formula         'C H Cl Cu N O S'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All N(H) groups, All O(H)
  groups
2. Restrained distances
 O2-H2
 0.85 with sigma of 0.02
 H3-N3
 0.85 with sigma of 0.02
 N2-H2A
 0.85 with sigma of 0.02
3. Others
 Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(N4A)=Sof(C40A)=1-FVAR(1)
 Sof(N4)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=FVAR(1)
4.a Riding coordinates:
 C39(H39A,H39B,H39C), C39(H39D,H39E,H39F)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C26(H26A,H26B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2B), C3(H3A), C4(H4), C5(H5), C7(H7), C14(H14), C15(H15), C16(H16),
 C17(H17), C21(H21), C22(H22), C23(H23), C28(H28), C29(H29), C30(H30), C31(H31),
  C35(H35), C36(H36), C37(H37), C44(H44)
4.d X=CH2 refined with riding coordinates:
 C43(H43A,H43B)
4.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              65336
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'