Are the metal identity and stoichiometry of metal complexes important for colchicine site binding and inhibition of tubulin polymerization?
Besleaga, Iuliana; Raptová, Renáta; Stoica, Alexandru-Constantin; Milunovic, Miljan N. M.; Zalibera, Michal; Bai, Ruoli; Igaz, Nóra; Reynisson, Jóhannes; Kiricsi, Mónika; Enyedy, Éva A; Rapta, Peter; Hamel, Ernest; Arion, Vladimir B.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12349–12369; doi:10.1039/d4dt01469c

data_7716514
_publ_section_title
;
 Are the metal identity and stoichiometry of metal complexes important for
 colchicine site binding and inhibition of tubulin polymerization?
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12349
_journal_page_last               12369
_journal_paper_doi               10.1039/d4dt01469c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C20 H24 N5 O2 S, N O3'
_chemical_formula_sum            'C20 H24 N6 O5 S'
_chemical_formula_weight         460.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-06-24
_audit_creation_method
;FinalCif V138 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-06-24 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.547(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9111(13)
_cell_length_b                   8.5430(6)
_cell_length_c                   18.0419(18)
_cell_measurement_reflns_used    18966
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.26
_cell_measurement_theta_min      3.93
_cell_volume                     2142.0(3)
_computing_cell_refinement
;
X-Area Recipe 2.0.1 (STOE, 2023)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.192.0 (STOE, 2023)
;
_computing_data_reduction
'  X-Area Integrate 2.5.15.0 (STOE, 2023)  X-Area LANA 2.7.12 (STOE, 2023)'
_computing_molecular_graphics    'ShelXle (H\"ubschle 2011)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.3, Darmstadt 2023
;
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'EIGER2 500K'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_details      ' 10614 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18583
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.638
_diffrn_reflns_theta_min         3.929
_diffrn_source                   'Primux 100 micro'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_T_max  0.9870
_exptl_absorpt_correction_T_min  0.5936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_exptl_crystal_size_rad          0.050
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3904
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1412P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1771
_refine_ls_wR_factor_ref         0.2007
_reflns_d_resolution_high        0.812
_reflns_d_resolution_low         18.024
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              7
_reflns_limit_l_min              -20
_reflns_number_gt                2649
_reflns_number_total             3904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01469c2.cif
_cod_data_source_block           IUBE4192_a
_cod_depositor_comments
'Adding full bibliography for 7716513--7716520.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7716514
_stoe_evaluation_lana_table
;----------------------------------------------------------------------------
2Theta          11.7   27.3   42.9   58.5   74.1   89.7  105.3  120.9  136.5
<Resolution>    6.59   3.08   2.08   1.57   1.26   1.10   0.97   0.89   0.83
N(total)          75   1035   1540   2122   2993   5024   4487   3611   2094
<Redundancy>     2.0    5.5    4.3    3.8    4.2    6.0    5.3    4.5    3.5
Complet. [%%]    93.9  100.0   97.1   95.2   92.8   94.7   93.1   92.3   80.1
<I/sigma>      178.6   71.4   30.4   14.7    6.2    4.8    2.7    2.6    2.6
R(int)         0.023  0.026  0.037  0.053  0.093  0.096  0.153  0.169  0.171
;
_stoe_evaluation_lana_mean_redundancy 4.7
_stoe_evaluation_lana_completeness 92.0
_stoe_evaluation_lana_number_refls_written 19236
_stoe_evaluation_lana_number_refls_unique 4134
_stoe_evaluation_lana_number_refls_after_or 19236
_stoe_evaluation_lana_number_refls_outliers 3745
_stoe_evaluation_lana_number_refls_total 22981
_stoe_evaluation_lana_max_2theta_desired 143.3
_stoe_evaluation_lana_max_2theta_available 143.3
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_point_group 2/m
_stoe_evaluation_integration_ems 0.028
_stoe_evaluation_integration_b   2.0
_stoe_evaluation_integration_a   12.7
_stoe_measurement_total_exposure_time '14.7 h'
_stoe_measurement_mean_exposure_per_frame '5.0 s'
_stoe_measurement_max_exposure_per_frame '5.0 s'
_stoe_measurement_min_exposure_per_frame '5.0 s'
_stoe_measurement_total_frame_number 10614
_stoe_measurement_total_run_number 99
_stoe_measurement_tube_power     '50.0 W'
_stoe_measurement_identifier     IUBE4192
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_size_y            '3.8 cm'
_stoe_detector_size_x            '7.7 cm'
_audit_contact_author            'J. Richter'
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.623
_shelx_estimated_absorpt_t_max   0.966
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              43944
_shelx_hkl_checksum              98844