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_7714482
_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         'C42 H28 Br2 Fe N6, 2(Br), 0.5(H2 O)'
_chemical_formula_sum            'C42 H29 Br4 Fe N6 O0.5'
_chemical_formula_weight         1001.20
_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             2023-11-11
_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                92.4960(10)
_cell_angle_beta                 90.3220(10)
_cell_angle_gamma                105.3680(10)
_cell_formula_units_Z            4
_cell_length_a                   8.74480(10)
_cell_length_b                   10.8183(2)
_cell_length_c                   42.8018(6)
_cell_measurement_reflns_used    23078
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.8450
_cell_measurement_theta_min      1.8960
_cell_volume                     3900.11(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.804
_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  0.0347
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.804
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            47575
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.804
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.454
_diffrn_reflns_theta_min         1.905
_exptl_absorpt_coefficient_mu    4.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro 1.171.42.89a'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       block
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.144
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1005
_refine_ls_number_reflns         17378
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0435P)^2^+16.9127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14004
_reflns_number_total             17378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02732e2.cif
_cod_data_source_block           febr14
_cod_original_formula_sum        'C42 H29 Br4 Fe N6 O0.50'
_cod_database_code               7714482
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.613
_shelx_estimated_absorpt_t_min   0.496
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Br1A-C19 \\sim Br1-C19
 with sigma of 0.02
 Br4A-C82 \\sim Br4-C82
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
4. Others
 Sof(Br1A)=Sof(Br7A)=Sof(Br8A)=1-FVAR(1)
 Sof(Br1)=Sof(Br7)=Sof(Br8)=FVAR(1)
 Sof(Br4A)=1-FVAR(2)
 Sof(Br4)=FVAR(2)
5.a Free rotating group:
 O1(H1A,H1B)
5.b 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), C22(H22), C23(H23), C24(H24),
  C25(H25), C28(H28), C30(H30), C33(H33), C34(H34), C35(H35), C36(H36),
 C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C49(H49), C51(H51), C54(H54), C55(H55), C56(H56), C57(H57), C59(H59),
 C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C70(H70),
  C72(H72), C75(H75), C76(H76), C77(H77), C78(H78), C80(H80), C81(H81),
 C83(H83), C84(H84)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              94896
_shelx_fab_checksum              79556
_olex2_submission_special_instructions 'No special instructions were received'