Rational design of a cytotoxic dinuclear cu2 complex that binds by molecular recognition at two neighboring phosphates of the DNA backbone.
Jany, Thomas; Moreth, Alexander; Gruschka, Claudia; Sischka, Andy; Spiering, Andre; Dieding, Mareike; Wang, Ying; Samo, Susan Haji; Stammler, Anja; Bögge, Hartmut; Fischer von Mollard, Gabriele; Anselmetti, Dario; Glaser, Thorsten; Inorganic chemistry 54 (2015) 2679–2690; doi:10.1021/ic5028465

data_4342336
_publ_section_title
;
 Rational design of a cytotoxic dinuclear cu2 complex that binds by
 molecular recognition at two neighboring phosphates of the DNA backbone.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2679
_journal_page_last               2690
_journal_paper_doi               10.1021/ic5028465
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H46 Cu2 N6 O6 , 9.75(H2 O) , C2 H3 N'
_chemical_formula_sum            'C46 H68.5 Cu2 N7 O15.75'
_chemical_formula_weight         1098.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9107(16)
_cell_length_b                   15.793(2)
_cell_length_c                   31.758(5)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      3.43
_cell_volume                     5472.3(14)
_computing_cell_refinement       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Bruker KAPPA APEX II'
_diffrn_measurement_device_type  'four circle diffractometer'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'graphite monochromator'
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            57003
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.8907
_exptl_absorpt_correction_T_min  0.7453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             2310
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         11883
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+0.1969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1243
_reflns_number_gt                10494
_reflns_number_total             11883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5028465_si_002.cif
_cod_data_source_block           g2000
_cod_depositor_comments          'Adding full bibliography for 4342336.cif.'
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_original_formula_sum        'C46 H68.50 Cu2 N7 O15.75'
_cod_database_code               4342336
_vrf
;
The compound crystallizes with 9.75 solvent water molecules per formula 
unit, which are disordered over 15 positions. The hydrogen atoms of 
these water molecules could not be located and refined. This accounts 
for all "checkcif" alerts of the type :
"Isolated Oxygen Atom (H-atoms Missing ?)",
"Isolated Disordered Oxygen Atom (No H's ?)", 
"Atom O14W    (Anion/Solvent) ADP max/min Ratio"
and for all alerts related to the difference between the reported 
and the calculated formula.
The alert "Low   'Solvent' Ueq as Compared to Neighbors of C2L" 
is probably caused by an unresolved slight disorder of the MeCN solvent 
molecule. 
;