Metal dipyrrin complexes as potential photosensitizers for photodynamic therapy
Karges, Johannes; Blacque, Olivier; Gasser, Gilles; Inorganica Chimica Acta 505 (2020) 119482–; doi:10.1016/j.ica.2020.119482

data_1565206
_publ_section_title
;
 Metal dipyrrin complexes as potential photosensitizers for photodynamic
 therapy
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119482
_journal_paper_doi               10.1016/j.ica.2020.119482
_journal_volume                  505
_journal_year                    2020
_chemical_formula_moiety         'C44 H46 I4 N4 Ni, 3(C H4 O)'
_chemical_formula_sum            'C47 H58 I4 N4 Ni O3'
_chemical_formula_weight         1293.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.6512(5)
_cell_length_b                   44.3536(14)
_cell_length_c                   17.5398(5)
_cell_measurement_reflns_used    5674
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      69.1600
_cell_measurement_theta_min      4.0470
_cell_volume                     11397.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_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   -130.00 -82.00   0.50   15.00    --  -54.72 -99.00-150.00   96
  2  \w   -130.00 -82.00   0.50   15.00    --  -54.72 -99.00 -30.00   96
  3  \w    -26.00  25.00   0.50   15.00    --  -54.72  19.00-150.00  102
  4  \w    -26.00  25.00   0.50   15.00    --  -54.72  19.00 -60.00  102
  5  \w    -26.00  25.00   0.50   15.00    --  -54.72  19.00 -90.00  102
  6  \w    -35.00  -6.00   0.50   60.00    --  -84.25  30.00  90.00   58
  7  \w     35.00  71.00   0.50   60.00    --  105.75 -61.00 120.00   72
  8  \w     36.00  64.00   0.50   60.00    --  105.75 -61.00  60.00   56
  9  \w     35.00  71.00   0.50   60.00    --  105.75 -61.00  30.00   72
 10  \w     35.00  71.00   0.50   60.00    --  105.75 -61.00   0.00   72
 11  \w     30.00 109.00   0.50   60.00    --  105.75 -94.00 -30.00  158
 12  \w     35.00  71.00   0.50   60.00    --  105.75 -61.00-180.00   72
 13  \w     59.00  99.00   0.50   60.00    --  105.75 -77.00-180.00   80
 14  \w     35.00  71.00   0.50   60.00    --  105.75 -61.00-120.00   72
 15  \w     94.00 178.00   0.50   60.00    --  105.75  45.00-120.00  168
 16  \w     99.00 178.00   0.50   60.00    --  105.75 111.00 120.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0132836000
_diffrn_orient_matrix_UB_12      0.0318789000
_diffrn_orient_matrix_UB_13      0.0331645000
_diffrn_orient_matrix_UB_21      -0.0683125000
_diffrn_orient_matrix_UB_22      -0.0126069000
_diffrn_orient_matrix_UB_23      0.0585060000
_diffrn_orient_matrix_UB_31      0.0788080000
_diffrn_orient_matrix_UB_32      -0.0056035000
_diffrn_orient_matrix_UB_33      0.0565017000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30356
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.493
_diffrn_reflns_theta_min         3.987
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.788
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.370
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       plate
_exptl_crystal_F_000             5056
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.225
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0666
_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^)+(0.1011P)^2^+44.6938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1863
_refine_ls_wR_factor_ref         0.2089
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3573
_reflns_number_total             5789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-505-119482.cif
_cod_data_source_block           1_sq
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               1565206
_shelx_estimated_absorpt_t_max   0.842
_shelx_estimated_absorpt_t_min   0.297
_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.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C18(H18)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;