Self-assembled Cu(ii) and Ni(ii) metallamacrocycles formed from 3,3,3',3'-tetrabenzyl-1,1'-aroylbis(thiourea) ligands: DNA and protein binding studies, and cytotoxicity of trinuclear complexes.
Selvakumaran, Nagamani; Bhuvanesh, Nattamai S. P.; Karvembu, Ramasamy; Dalton transactions (Cambridge, England : 2003) 43 (2014) 16395–16410; doi:10.1039/c4dt01859a

data_7032227
_publ_section_title
;
 Self-assembled Cu(ii) and Ni(ii) metallamacrocycles formed from
 3,3,3',3'-tetrabenzyl-1,1'-aroylbis(thiourea) ligands: DNA and protein
 binding studies, and cytotoxicity of trinuclear complexes.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16395
_journal_page_last               16410
_journal_paper_doi               10.1039/c4dt01859a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C86 H74 Cu2 N10 O4 S4, 5(C5 H5 N)'
_chemical_formula_sum            'C111 H99 Cu2 N15 O4 S4'
_chemical_formula_weight         1962.37
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-03-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.672(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.901(2)
_cell_length_b                   38.112(8)
_cell_length_c                   12.697(3)
_cell_measurement_reflns_used    9614
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      27.448
_cell_measurement_theta_min      2.336
_cell_volume                     4793.5(18)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            66701
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         1.844
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0521 before and 0.0482 after correction.
The Ratio of minimum to maximum transmission is 0.9406.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         10961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0297P)^2^+4.2398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9288
_reflns_number_total             10961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01859a2.cif
_cod_data_source_block           cu
_cod_depositor_comments
'Adding full bibliography for 7032224--7032227.cif.'
_cod_original_cell_volume        4793.5(17)
_cod_database_code               7032227
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.875
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{N13P, C13P}
3. Uiso/Uaniso restraints and constraints
Uanis(N13P) = Uanis(C13P)
4. Others
 Fixed Sof: N13P(0.5) C13P(0.5) H13P(0.5)
5.a Riding coordinates:
 C13P(H13P), C14P(H14P), C15P(H15P)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C15(H15A,H15B), C30(H30A,H30B), C37(H37A,H37B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
  C24(H24), C25(H25), C27(H27), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C2P(H2P), C3P(H3P),
  C4P(H4P), C5P(H5P), C6P(H6P), C8P(H8P), C9P(H9P), C10P(H10P), C11P(H11P),
 C12P(H12P)
;
_shelx_res_checksum              37271