Metal complexes of pro-vitamin K3 analog phthiocol (2-hydroxy-3-methylnaphthalene-1,4-dione): Synthesis, Characterization and anticancer activity
Harihar, Shital; Mone, Nishigandha Sanjay; Satpute, Surekha Khandu; Chadar, Dattatray; Chakravarty, Debamitra; Weyhermueller, Thomas; Butcher, R. J.; Salunke-Gawali, Sunita; Dalton Transactions  (2022) –; doi:10.1039/D2DT02748H

data_7711476
_publ_section_title
;
 Metal complexes of pro-vitamin K3 analog phthiocol
 (2-hydroxy-3-methylnaphthalene-1,4-dione): Synthesis, Characterization
 and anticancer activity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02748H
_journal_year                    2022
_chemical_formula_moiety         'C48 H48 Ni4 O20, 4(H2O)'
_chemical_formula_sum            'C48 H56 Ni4 O24'
_chemical_formula_weight         1251.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-23 deposited with the CCDC.	2022-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.062(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.133(3)
_cell_length_b                   12.8402(19)
_cell_length_c                   21.624(3)
_cell_measurement_reflns_used    9206
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.36
_cell_measurement_theta_min      2.74
_cell_volume                     5299.1(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2230
_diffrn_reflns_av_unetI/netI     0.1385
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50722
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         2.634
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  0.8818
_exptl_absorpt_correction_T_min  0.6062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         4936
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1882
_refine_ls_R_factor_gt           0.0991
_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^)+(0.0649P)^2^+105.3469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2334
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2722
_reflns_number_total             4936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02748h2.cif
_cod_data_source_block           shelx_CCDC4
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7711476
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              2878