Fe(II) complexes of 2,2':6',2"-terpyridine ligands functionalized with substituted-phenyl groups: Synthesis, crystal structures and anticancer potential
Sun, Dameng; Huang, Xin; Man, Ruo-Jun; Jia, Xinjie; Song, Xinluan; Wang, Sihan; Xue, Xingyong; Liu, Hongming; Ma, Zhen; Dalton Transactions  (2023) –; doi:10.1039/D3DT02732E

data_7714481
_publ_section_title
;
 Fe(II) complexes of 2,2':6',2"-terpyridine ligands functionalized with
 substituted-phenyl groups: Synthesis, crystal structures and anticancer
 potential
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02732E
_journal_year                    2023
_chemical_formula_moiety         '2(Br), Br3, 2(C44 H30 Fe N6 O4), 4(H2 O)'
_chemical_formula_sum            'C88 H68 Br5 Fe2 N12 O12'
_chemical_formula_weight         1996.79
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-12
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2023-11-12 deposited with the CCDC.	2023-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                83.6260(10)
_cell_angle_beta                 76.9870(10)
_cell_angle_gamma                87.4980(10)
_cell_formula_units_Z            1
_cell_length_a                   9.26360(10)
_cell_length_b                   12.0848(2)
_cell_length_c                   19.0429(3)
_cell_measurement_reflns_used    13796
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.6010
_cell_measurement_theta_min      1.7060
_cell_volume                     2063.86(5)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.806
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.806
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25736
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.392
_diffrn_reflns_theta_min         1.696
_exptl_absorpt_coefficient_mu    2.842
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60709
_exptl_absorpt_process_details   'CrysAlisPro 1.171.42.89a'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             1003
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.571
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         9196
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0467P)^2^+6.2427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7866
_reflns_number_total             9196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02732e2.cif
_cod_data_source_block           febr11
_cod_depositor_comments
;

2024-11-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         998.39
_cod_original_formula_moiety         '1.667(Br1.5), C44 H30 Fe N6 O4, 2(H2 O)'
_cod_original_formula_units_Z            2
_cod_original_formula_sum        'C44 H34 Br2.50 Fe N6 O6'
_cod_database_code               7714481
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.745
_shelx_estimated_absorpt_t_min   0.692
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H2-O2
 0.85 with sigma of 0.01
3.a Riding coordinates:
 O2(H2)
3.b Free rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3), C4(H4A), C7(H7), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24),
  C25(H25), C26(H26), C29(H29), C31(H31), C34(H34), C35(H35), C36(H36),
 C37(H37), C39(H39), C40(H40), C42(H42), C43(H43)
3.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              282
_shelx_fab_checksum              50983
_olex2_submission_special_instructions 'No special instructions were received'