A simple and feasible atom-precise biotinylated Cu(i) complex for tumor-targeted chemodynamic therapy.
Luo, Bi; Chen, Liguang; Hong, Zhaoguo; You, Xin; Huang, Fu-Ping; Bian, He-Dong; Zhang, Liangliang; Zhao, Shulin; Chemical communications (Cambridge, England) 57 (2021) 6046–6049; doi:10.1039/d1cc00515d

data_7128320
_publ_section_title
;
 A simple and feasible atom-precise biotinylated Cu(i) complex for
 tumor-targeted chemodynamic therapy.
;
_journal_issue                   49
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6046
_journal_page_last               6049
_journal_paper_doi               10.1039/d1cc00515d
_journal_volume                  57
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H32 Cl Cu N4 O6 S2'
_chemical_formula_sum            'C20 H32 Cl Cu N4 O6 S2'
_chemical_formula_weight         587.60
_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_Hall           'I 4bw'
_space_group_name_H-M_alt        'I 41'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-25 deposited with the CCDC.	2021-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.3667(5)
_cell_length_b                   37.3667(5)
_cell_length_c                   4.75497(13)
_cell_measurement_reflns_used    8076
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.3530
_cell_measurement_theta_min      3.8380
_cell_volume                     6639.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9784
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -12.00  88.00   0.50   25.00    --   17.77  77.00  30.00  200
  2  \w    -12.00  88.00   0.50   25.00    --   17.77  77.00-120.00  200
  3  \w    -88.00   2.00   0.50   25.00    --  -19.57 -57.00  30.00  180
  4  \w    -41.00  49.00   0.50   25.00    --  -19.57  57.00 -60.00  180
  5  \w    -50.00  51.00   0.50   25.00    --  -19.57  77.00 150.00  202
  6  \w     34.00  94.00   0.50   25.00    --   17.77-178.00 120.00  120
  7  \w    -88.00   2.00   0.50   25.00    --  -19.57 -57.00 150.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0006914000
_diffrn_orient_matrix_UB_12      0.0189341000
_diffrn_orient_matrix_UB_13      -0.0089548000
_diffrn_orient_matrix_UB_21      -0.0189625000
_diffrn_orient_matrix_UB_22      -0.0006694000
_diffrn_orient_matrix_UB_23      0.0031921000
_diffrn_orient_matrix_UB_31      0.0003647000
_diffrn_orient_matrix_UB_32      0.0011473000
_diffrn_orient_matrix_UB_33      0.1489071000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            40617
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         3.271
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 1398 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         6758
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1218P)^2^+2.1298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1961
_refine_ls_wR_factor_ref         0.2220
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4663
_reflns_number_total             6758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00515d2.cif
_cod_data_source_block           20200507-hfp-lb-n9-cu1aaa_sq
_cod_depositor_comments          'Adding full bibliography for 7128320.cif.'
_cod_original_cell_volume        6639.2(3)
_cod_database_code               7128320
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.841
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C20-O5' \\sim C20-O6' \\sim C20-O5 \\sim C20-O6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq, Uanis(Cl1') \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(O5') \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O6') \\sim Ueq, Uanis(O5)
\\sim Ueq, Uanis(Cu1') \\sim Ueq, Uanis(Cu1) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5') = Uanis(O6) = Uanis(O5) = Uanis(O6')
4. Others
 Sof(Cu1)=Sof(Cl1)=1-FVAR(1)
 Sof(Cu1')=Sof(Cl1')=FVAR(1)
 Sof(O5)=Sof(O6)=Sof(H6A)=1-FVAR(2)
 Sof(O5')=Sof(H5')=Sof(O6')=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C6(H6), C7(H7), C9(H9), C14(H14), C12(H12)
5.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2A,H2B), C5(H5A,H5B), C10(H10A,H10B), C16(H16A,H16B), C3(H3A,
 H3B), C11(H11A,H11B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N4(H4), N1(H1A)
5.d Tetrahedral OH refined with riding coordinates:
 O1(H1), O5'(H5'), O6(H6A)
;
_shelx_res_checksum              19010
_shelx_fab_checksum              46576
_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 2.182
_oxdiff_exptl_absorpt_empirical_full_min 0.540