Two novel chiral tetranucleate copper-based complexes: syntheses, crystal structures, inhibition of angiogenesis and the growth of human breast cancer in vitro and in vivo
Hou, Xiao-Xiao; Ren, Ya-Ping; Luo, Zhao-Hui; Jiang, Bing-Li; Lu, Tian-Tian; Huang, Fu-Ping; Qin, Xiu-Ying; Dalton Transactions  (2021) –; doi:10.1039/D1DT02033A

data_7708461
_publ_section_title
;
 Two novel chiral tetranucleate copper-based complexes: syntheses, crystal
 structures, inhibition of angiogenesis and the growth of human breast
 cancer in vitro and in vivo
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02033A
_journal_year                    2021
_chemical_formula_moiety         'C80 H124 Cu4 N4 O8 S4'
_chemical_formula_sum            'C80 H124 Cu4 N4 O8 S4'
_chemical_formula_weight         1652.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-28 deposited with the CCDC.	2021-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.102(5)
_cell_length_b                   11.779(2)
_cell_length_c                   14.489(3)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.033
_cell_measurement_theta_min      2.228
_cell_volume                     4454.7(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33587
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.386
_diffrn_reflns_theta_min         1.405
_exptl_absorpt_coefficient_mu    1.086
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 2988 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         9077
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0878P)^2^+0.7380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1370
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                7546
_reflns_number_total             9077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02033a2.cif
_cod_data_source_block           zxy1
_cod_original_cell_volume        4454.7(16)
_cod_database_code               7708461
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.928
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S2A-C25 = S2-C25A
 1.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(C4) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C2A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(S1) \\sim Ueq,
Uanis(S1A) \\sim Ueq, Uanis(S2A) \\sim Ueq, Uanis(S2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C25) = Uanis(C25A)
Uanis(C1) = Uanis(C1A)
Uanis(C24) = Uanis(C24A)
Uanis(S1) = Uanis(S1A)
Uanis(C2) = Uanis(C2A)
Uanis(C3) = Uanis(C3A)
Uanis(C4) = Uanis(C4A)
Uanis(S2) = Uanis(S2A)
4. Others
 Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=FVAR(1)
 Sof(H5BC)=Sof(H5BD)=Sof(C4A)=Sof(H4A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=1-FVAR(2)
 Sof(H5AA)=Sof(H5AB)=Sof(C4)=Sof(H4)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=FVAR(2)
 Sof(S1A)=1-FVAR(3)
 Sof(S1)=FVAR(3)
 Sof(S2A)=1-FVAR(4)
 Sof(S2)=FVAR(4)
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(5)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(5)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(6)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(6)
5.a Ternary CH refined with riding coordinates:
 C22(H22), C4(H4), C4A(H4A)
5.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C5(H5AA,H5AB), C5(H5BC,H5BD), C23(H23A,H23B), C23(H23C,H23D),
 C3(H3A,H3B), C2(H2A,H2B), C24(H24A,H24B), C24A(H24C,H24D), C3A(H3AA,H3AB),
 C2A(H2AA,H2AB)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C26(H26), C10(H10), C30(H30), C6(H6), C32(H32)
5.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C19(H19A,H19B,H19C), C36(H36A,H36B,H36C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C34(H34A,H34B,H34C), C15(H15A,H15B,H15C), C20(H20A,
 H20B,H20C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C14(H14A,H14B,H14C),
 C40(H40A,H40B,H40C), C1(H1A,H1B,H1C), C25(H25A,H25B,H25C), C25A(H25D,H25E,
 H25F), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              15472
_shelx_hkl_checksum              20820
_olex2_submission_special_instructions 'No special instructions were received'