Mn(III), Zn(II) and Pt(II) macroacyclic complexes: Synthesis, X-ray structures, anticancer and antioxidant activities
Keypour, Hassan; Ansari, Neda; Mahmoudabadi, Masoumeh; Karamian, Roya; Moazzami Farida, Seyed Hamed; Eslami Moghadam, Mahboube; William Gable, Robert; Inorganica Chimica Acta 509 (2020) 119705–; doi:10.1016/j.ica.2020.119705

data_1564472
_publ_section_title
;
 Mn(III), Zn(II) and Pt(II) macroacyclic complexes: Synthesis, X-ray
 structures, anticancer and antioxidant activities
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119705
_journal_paper_doi               10.1016/j.ica.2020.119705
_journal_volume                  509
_journal_year                    2020
_chemical_formula_moiety         'C18 H24 N4 Pt, 1.535(Cl), 0.465(I)'
_chemical_formula_sum            'C18 H24 Cl1.535 I0.465 N4 Pt'
_chemical_formula_weight         604.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 96.669(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4651(4)
_cell_length_b                   16.0394(6)
_cell_length_c                   11.9601(4)
_cell_measurement_reflns_used    5752
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      31.7530
_cell_measurement_theta_min      3.3940
_cell_volume                     1993.97(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -53.00  44.00   1.00   12.48    --   17.98 -57.00  90.00   97
  2  \w     -5.00  89.00   1.00   12.48    --   17.98  57.00-120.00   94
  3  \w    -91.00   8.00   1.00   12.48    --  -18.60 -77.00 -30.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0488520000
_diffrn_orient_matrix_UB_12      -0.0002452000
_diffrn_orient_matrix_UB_13      0.0364415000
_diffrn_orient_matrix_UB_21      -0.0462679000
_diffrn_orient_matrix_UB_22      -0.0104469000
_diffrn_orient_matrix_UB_23      -0.0459971000
_diffrn_orient_matrix_UB_31      0.0115135000
_diffrn_orient_matrix_UB_32      -0.0429640000
_diffrn_orient_matrix_UB_33      0.0109647000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17514
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.319
_diffrn_reflns_theta_min         2.750
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.971
_exptl_absorpt_correction_T_max  0.559
_exptl_absorpt_correction_T_min  0.155
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_description       needle
_exptl_crystal_F_000             1155
_exptl_crystal_recrystallization_method
'crystallized by slow evaporation from ethanol'
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.174
_refine_diff_density_max         1.573
_refine_diff_density_min         -1.943
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         6540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0150P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0491
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5560
_reflns_number_total             6540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rwg2019_16bGau.cif
_cod_data_source_block           rwg2019_16bgau
_cod_original_cell_volume        1993.96(13)
_cod_database_code               1564472
_chemical_oxdiff_formula         'C18 H24 Cl1.5 I0.5 N4 Pt'
_chemical_oxdiff_usercomment     MAH2
_shelx_estimated_absorpt_t_max   0.338
_shelx_estimated_absorpt_t_min   0.197
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(I1) = Uanis(Cl1)
Uanis(I2) = Uanis(Cl2)
3. Others
 Sof(I1)=1-FVAR(1)
 Sof(Cl1)=FVAR(1)
 Sof(I2)=1-FVAR(2)
 Sof(Cl2)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C14(H14), C15(H15), C16(H16), C17(H17)
;
_shelx_res_checksum              45126
_shelx_hkl_checksum              74238
_olex2_exptl_crystal_mounting_method 'mounted on a cryoloop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.428
_oxdiff_exptl_absorpt_empirical_full_min 0.637