Two novel chiral tetranucleate copper-based complexes: crystal structures, nanoparticles, and inhibiting angiogenesis and the growth of human breast cancer by regulating the VEGF/VEGFR2 signal pathway in vitro.
Zhang, Pei-Lu; Hou, Xiao-Xiao; Liu, Mei-Rong; Huang, Fu-Ping; Qin, Xiu-Ying; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6043–6055; doi:10.1039/d0dt00380h

data_7703987
_publ_section_title
;
 Two novel chiral tetranucleate copper-based complexes: crystal
 structures, nanoparticles, and inhibiting angiogenesis and the growth of
 human breast cancer by regulating the VEGF/VEGFR2 signal pathway in
 vitro.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6043
_journal_page_last               6055
_journal_paper_doi               10.1039/d0dt00380h
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H52 Br4 Cl4 Cu4 N4 O8 S4, 2(H2 O)'
_chemical_formula_sum            'C48 H56 Br4 Cl4 Cu4 N4 O10 S4'
_chemical_formula_weight         1692.81
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-03-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                85.732(3)
_cell_angle_beta                 84.872(3)
_cell_angle_gamma                85.986(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1515(3)
_cell_length_b                   13.6106(4)
_cell_length_c                   22.1971(9)
_cell_measurement_reflns_used    5810
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3430
_cell_measurement_theta_min      3.6230
_cell_volume                     3039.98(18)
_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  'ShelXH-1997 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     -5.00  22.00   1.00    7.00    --   18.63 -99.00-150.00   27
  2  \w     19.00  57.00   1.00    7.00    --   18.63 -99.00 150.00   38
  3  \w    -12.00  61.00   1.00    7.00    --   18.63 -99.00 -90.00   73
  4  \w    -63.00  45.00   1.00    7.00    --  -18.94  19.00 150.00  108
  5  \w    -69.00  25.00   1.00    7.00    --  -18.94 -19.00  90.00   94
  6  \w    -74.00  11.00   1.00    7.00    --  -18.94 -77.00   0.00   85
;
_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      -0.0032104000
_diffrn_orient_matrix_UB_12      -0.0332451000
_diffrn_orient_matrix_UB_13      -0.0228859000
_diffrn_orient_matrix_UB_21      -0.0107183000
_diffrn_orient_matrix_UB_22      -0.0389523000
_diffrn_orient_matrix_UB_23      0.0225906000
_diffrn_orient_matrix_UB_31      -0.0693992000
_diffrn_orient_matrix_UB_32      0.0109366000
_diffrn_orient_matrix_UB_33      0.0003259000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24959
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.29
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.378
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1680
_refine_diff_density_max         1.860
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1425
_refine_ls_number_reflns         20039
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1810
_reflns_number_gt                14762
_reflns_number_total             20039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt00380h2.cif
_cod_data_source_block           m20180927-1
_cod_depositor_comments
;
Adding full bibliography for 7703986--7703987.cif.

2024-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C48 H52 Br4 Cl4 Cu4 N4 O8 S4), 4(H2 O)'
_cod_original_formula_sum        'C96 H112 Br8 Cl8 Cu8 N8 O20 S8'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     3385.62
_cod_database_code               7703987
_chemical_oxdiff_formula         'C1 H1 O1 N1 S1 Br1 Cl1 Cu1'
_reflns_odcompleteness_completeness 99.76
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C60-S5
 1.8 with sigma of 0.01
 C36-S3
 1.8 with sigma of 0.01
 C12-S1
 1.8 with sigma of 0.02
 O2-C8
 1.42 with sigma of 0.001
 C20-O4
 1.42 with sigma of 0.001
 C56-O10
 1.42 with sigma of 0.001
 C92-O16
 1.42 with sigma of 0.001
3. Rigid bond restraints
 S5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C60, S5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C36) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.01
5.a Free rotating group:
 O4W(H4WA,H4WB), O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
5.b Ternary CH refined with riding coordinates:
 C81(H81), C21(H21), C69(H69), C57(H57), C93(H93), C9(H9), C33(H33), C45(H45)
5.c Secondary CH2 refined with riding coordinates:
 C80(H80A,H80B), C8(H8A,H8B), C92(H92A,H92B), C56(H56A,H56B), C70(H70A,H70B),
 C32(H32A,H32B), C94(H94A,H94B), C59(H59A,H59B), C82(H82A,H82B), C22(H22A,H22B),
  C68(H68A,H68B), C58(H58A,H58B), C20(H20A,H20B), C95(H95A,H95B), C44(H44A,
 H44B), C46(H46A,H46B), C83(H83A,H83B), C10(H10A,H10B), C47(H47A,H47B),
 C71(H71A,H71B), C23(H23A,H23B), C34(H34A,H34B), C35(H35A,H35B), C11(H11A,H11B)
5.d Aromatic/amide H refined with riding coordinates:
 C19(H19), C52(H52), C43(H43), C55(H55), C67(H67), C76(H76), C74(H74),
 C90(H90), C31(H31), C62(H62), C16(H16), C50(H50), C6(H6), C30(H30), C79(H79),
 C91(H91), C64(H64), C4(H4), C7(H7), C18(H18), C28(H28), C40(H40), C88(H88),
 C42(H42)
5.e Idealised Me refined as rotating group:
 C72(H72A,H72B,H72C), C96(H96A,H96B,H96C), C84(H84A,H84B,H84C), C48(H48A,H48B,
 H48C), C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C60(H60A,H60B,H60C), C36(H36A,
 H36B,H36C)
;
_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 1.414
_oxdiff_exptl_absorpt_empirical_full_min 0.778