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_7714480
_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), C44 H34 Fe N6 O4 S2'
_chemical_formula_sum            'C44 H34 Br2 Fe N6 O4 S2'
_chemical_formula_weight         990.56
_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   geom
_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                79.159(11)
_cell_angle_beta                 85.249(10)
_cell_angle_gamma                75.473(11)
_cell_formula_units_Z            2
_cell_length_a                   8.8732(10)
_cell_length_b                   15.936(2)
_cell_length_c                   16.198(2)
_cell_measurement_reflns_used    1325
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.0770
_cell_measurement_theta_min      4.0250
_cell_volume                     2176.1(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      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0912
_diffrn_reflns_av_unetI/netI     0.2002
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15311
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.427
_exptl_absorpt_coefficient_mu    2.328
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93644
_exptl_absorpt_process_details   'CrysAlisPro 1.171.38.41'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         7679
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.2022
_refine_ls_R_factor_gt           0.0902
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0935P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1876
_refine_ls_wR_factor_ref         0.2516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3309
_reflns_number_total             7679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02732e2.cif
_cod_data_source_block           febr_8
_cod_original_cell_volume        2176.2(5)
_cod_database_code               7714480
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.693
_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
2. Restrained distances
 S0-O4A \\sim S006-O4
 with sigma of 0.02
 S0-C41 \\sim S006-C41
 with sigma of 0.02
 S0-O3A \\sim S006-O3
 with sigma of 0.02
 S0-C44A \\sim S006-C44
 with sigma of 0.02
 O4-O3 \\sim O4A-O3A
 with sigma of 0.02
 O4-C44 \\sim O4A-C44A
 with sigma of 0.02
 O3-C44 \\sim O3A-C44A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S006 \\sim O3 \\sim O4 \\sim C41 \\sim C44: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
S0 \\sim O3A \\sim O4A \\sim C41 \\sim C44A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(C44) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(C44A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 S006, O3, O4, C41, C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 S0, O3A, O4A, C41, C44A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(S0)=Sof(O3A)=Sof(O4A)=Sof(C44A)=Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(1)
 Sof(S006)=Sof(O3)=Sof(O4)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(1)
 Fixed Sof: Br1(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), 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)
6.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C44(H44A,H44B,H44C), C44A(H44D,H44E,H44F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              33021
_shelx_fab_checksum              36765
_olex2_submission_special_instructions 'No special instructions were received'