Cytotoxic heteroleptic heptacoordinate salan zirconium(iv)-bis-chelates - synthesis, aqueous stability and X-ray structure analysis.
Schneider, Fabian; Zhao, Tiankun; Huhn, Thomas; Chemical communications (Cambridge, England) 52 (2016) 10151–10154; doi:10.1039/c6cc05359a

data_7124890
_publ_section_title
;
 Cytotoxic heteroleptic heptacoordinate salan zirconium(iv)-bis-chelates -
 synthesis, aqueous stability and X-ray structure analysis.
;
_journal_issue                   66
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10151
_journal_page_last               10154
_journal_paper_doi               10.1039/c6cc05359a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C44 H60 N4 O4 Zr, C1 H2 Cl2'
_chemical_formula_sum            'C45 H62 Cl2 N4 O4 Zr'
_chemical_formula_weight         885.10
_chemical_melting_point          566
_chemical_properties_physical    ', Moisture-sensitive'
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-07-20 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.342(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9667(6)
_cell_length_b                   18.0916(8)
_cell_length_c                   18.8976(9)
_cell_measurement_reflns_used    32141
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      1.83
_cell_volume                     4413.9(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1086
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52900
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.834
_diffrn_reflns_theta_min         1.561
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_T_max  0.9487
_exptl_absorpt_correction_T_min  0.6603
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methylenchloride, hexane'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.084
_refine_diff_density_min         -1.501
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         9388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+5.9952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7847
_reflns_number_total             9388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05359a2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7124890
_shelxl_version_number           2013-4
_shelx_res_checksum              10433