A β-carboline derivative-based nickel(ii) complex as a potential antitumor agent: synthesis, characterization, and cytotoxicity.
Yang, Jing-Mei; Zhu, Yan-Hong; Chen, Sheng; Lu, Xing; Wu, Yi-Ming; Ma, Feng-E; Li, Liang-Ping; Yang, Yang; Shi, Zhen-Hao; Huang, Kun-Yuan; Hong, Xue; Jiang, Ping; Peng, Yan; MedChemComm 9 (2018) 100–107; doi:10.1039/c7md00428a

data_7120919
_publ_section_title
;
 A \b-carboline derivative-based nickel(ii) complex as a potential
 antitumor agent: synthesis, characterization, and cytotoxicity.
;
_journal_issue                   1
_journal_name_full               MedChemComm
_journal_page_first              100
_journal_page_last               107
_journal_paper_doi               10.1039/c7md00428a
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C35 H29 N7 Ni O6, N O3, 0.5(O), 0.5(C2 H6 O)'
_chemical_formula_sum            'C36 H33 N8 Ni O10'
_chemical_formula_weight         795.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1n5zwp
_audit_creation_date             2015-03-25
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_audit_update_record
;
2017-08-19 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.640(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.435(2)
_cell_length_b                   19.1274(19)
_cell_length_c                   22.985(3)
_cell_measurement_reflns_used    2182
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.9920
_cell_measurement_theta_min      3.4550
_cell_volume                     7173.2(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_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 0.8663
_diffrn_measured_fraction_theta_max 0.6410
_diffrn_measurement_details
;
  1 omega  -94.00  -35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9263 -178.0000    0.0000 59

  2 omega  -91.00   26.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9263  -19.0000 -120.0000 117

  3 omega  -87.00   13.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9263    0.0000   30.0000 100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0121169000
_diffrn_orient_matrix_UB_12      0.0007714000
_diffrn_orient_matrix_UB_13      -0.0328584000
_diffrn_orient_matrix_UB_21      -0.0047482000
_diffrn_orient_matrix_UB_22      0.0368760000
_diffrn_orient_matrix_UB_23      0.0003575000
_diffrn_orient_matrix_UB_31      0.0414902000
_diffrn_orient_matrix_UB_32      0.0044239000
_diffrn_orient_matrix_UB_33      0.0026466000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.1613
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18952
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.32
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3300
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.20(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         11081
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1813
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          4.697
_refine_ls_shift/su_mean         0.255
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1877
_reflns_number_gt                4570
_reflns_number_total             11081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7md00428a2.cif
_cod_data_source_block           0313-py-zyh-wkl-nin
_cod_depositor_comments
;

2018-02-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 7120919.cif.
;
_cod_original_cell_volume        7173.1(14)
_cod_original_formula_moiety
'C35 H29 N7 Ni O6, C35 H30 N8 Ni O9, N O3, O, C2 H6 O'
_cod_original_formula_sum        'C72 H65 N16 Ni2 O20'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1591.82
_cod_database_code               7120919
_reflns_odcompleteness_completeness 86.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32