Mitochondria-localizing dicarbohydrazide Ln complexes and their mechanism of in vitro anticancer activity.
Meng, Ting; Liu, Tong; Qin, Qi-Pin; Chen, Zi-Lu; Zou, Hua-Hong; Wang, Kai; Liang, Fu-Pei; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4404–4415; doi:10.1039/d0dt00210k

data_7703733
_publ_section_title
;
 Mitochondria-localizing dicarbohydrazide Ln complexes and their mechanism
 of in vitro anticancer activity.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4404
_journal_page_last               4415
_journal_paper_doi               10.1039/d0dt00210k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C67 H57 Dy5 N12 O23, 2(H2 O)'
_chemical_formula_sum            'C67 H61 Dy5 N12 O25'
_chemical_formula_weight         2246.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-01-11 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                108.286(2)
_cell_angle_beta                 95.0240(10)
_cell_angle_gamma                102.3810(10)
_cell_formula_units_Z            2
_cell_length_a                   15.4027(2)
_cell_length_b                   15.9505(3)
_cell_length_c                   19.8366(4)
_cell_measurement_reflns_used    28129
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.8380
_cell_measurement_theta_min      2.3590
_cell_volume                     4456.31(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54969
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.583
_diffrn_reflns_theta_min         2.379
_exptl_absorpt_coefficient_mu    22.630
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       block
_exptl_crystal_F_000             2154
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.817
_exptl_transmission_factor_min   0.528
_refine_diff_density_max         1.920
_refine_diff_density_min         -1.745
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         18000
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0621P)^2^+33.7486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15556
_reflns_number_total             18000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00210k2.cif
_cod_data_source_block           222_sq
_cod_depositor_comments
'Adding full bibliography for 7703732--7703737.cif.'
_cod_database_code               7703733
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.211
_shelx_estimated_absorpt_t_min   0.056
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O19-H19
 0.85 with sigma of 0.01
 H24A-H19
 2.2 with sigma of 0.02
 H25B-H22B
 2.2 with sigma of 0.02
 C59-C60
 1.665 with sigma of 0.02
 C60-C59
 1.7 with sigma of 0.02
 H31_$1-H59C_$2
 2.2 with sigma of 0.02
 H20-O20
 0.82 with sigma of 0.02
 O21-H21
 0.82 with sigma of 0.02
 H21-O21
 0.85 with sigma of 0.02
 H21-Dy2
 2.6 with sigma of 0.02
 C67-H19
 1.896305 with sigma of 0.02
 Dy2-H19
 2.898714 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C67) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Free rotating group:
 O24(H24A,H24B), O25(H25A,H25B)
4.b Rotating group:
 O22(H22A,H22B), O23(H23A,H23B)
4.c Aromatic/amide H refined with riding coordinates:
 C47(H47), C10(H10), C45(H45), C44(H44), C35(H35), C38(H38), C50(H50),
 C19(H19A), C46(H46), C30(H30), C55(H55), C39(H39), C16(H16), C17(H17),
 C52(H52), C2(H2), C54(H54), C7(H7), C11(H11), C31(H31), C27(H27), C18(H18),
 C53(H53), C26(H26), C3(H3), C5(H5), C24(H24), C22(H22), C33(H33), C25(H25),
 C4(H4), C32(H32)
4.d Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C65(H65A,H65B,H65C), C61(H61A,H61B,H61C), C67(H67A,H67B,
 H67C), C57(H57A,H57B,H57C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              81172
_shelx_fab_checksum              76073
_olex2_submission_special_instructions 'No special instructions were received'