Synthesis, structure and properties of coordination complexes of tin(ii) phthalocyanine and naphthalocyanine with transition metal fragments
Faraonov, Maxim A.; Yudanova, Evgeniya I.; Kuzmin, Alexey V.; Khasanov, Salavat S.; Troyanov, Sergey I.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Konarev, Dmitri V.; CrystEngComm 25 (2023) 4620–4637; doi:10.1039/D3CE00564J

data_7247033
_publ_section_title
;
 Synthesis, structure and properties of coordination complexes of tin(ii)
 phthalocyanine and naphthalocyanine with transition metal fragments
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4620
_journal_page_last               4637
_journal_paper_doi               10.1039/D3CE00564J
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C42 H31 Cl2 Ir N8 Sn'
_chemical_formula_sum            'C42 H31 Cl2 Ir N8 Sn'
_chemical_formula_weight         1029.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-14
_audit_creation_method
;
FinalCif V119 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2023-05-21 deposited with the CCDC.	2023-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.808(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8043(8)
_cell_length_b                   11.4261(7)
_cell_length_c                   25.2186(17)
_cell_measurement_reflns_used    4043
_cell_measurement_temperature    100.0(8)
_cell_measurement_theta_max      25.9550
_cell_measurement_theta_min      1.6380
_cell_volume                     3582.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.856
_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     21.00 103.50   0.75  100.00    --   16.58  19.00  60.00  110
  2  \w    -10.00  16.25   0.75  100.00    --   16.58  19.00  60.00   35
  3  \w    -39.00 -12.00   0.75  100.00    --  -16.73 -60.00  35.71   36
  4  \w    -52.00 -25.00   0.75  100.00    --  -16.73  57.00 -60.00   36
  5  \w    -79.00  -1.00   0.75  100.00    --  -16.73 -60.00 121.68  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0271532000
_diffrn_orient_matrix_UB_12      0.0455054000
_diffrn_orient_matrix_UB_13      -0.0169289000
_diffrn_orient_matrix_UB_21      0.0420714000
_diffrn_orient_matrix_UB_22      0.0393999000
_diffrn_orient_matrix_UB_23      0.0116803000
_diffrn_orient_matrix_UB_31      0.0272713000
_diffrn_orient_matrix_UB_32      -0.0152636000
_diffrn_orient_matrix_UB_33      -0.0204010000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.1532
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            18772
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.021
_diffrn_reflns_theta_min         1.638
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.698
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         8183
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0724
_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^)+(0.0304P)^2^+7.6738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1364
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5240
_reflns_number_total             8183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00564j2.cif
_cod_data_source_block           PMCpIrCl2SnPc
_cod_depositor_comments
'Adding full bibliography for 7247026--7247038.cif.'
_cod_database_code               7247033
_chemical_oxdiff_formula         'C66 H34 Ir Cl2 Sn O6'
_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. Uiso/Uaniso restraints and constraints
C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106 \\sim C107 \\sim
C108 \\sim C109 \\sim C110 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim
C115 \\sim C116 \\sim C117 \\sim C118 \\sim C119 \\sim C120 \\sim C121 \\sim
C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126 \\sim C127 \\sim C128 \\sim
C129 \\sim C130 \\sim C131 \\sim C132 \\sim C201 \\sim C202 \\sim C203 \\sim
C204 \\sim C205 \\sim C206 \\sim C207 \\sim C208 \\sim C209 \\sim C210: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
3.a Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105), C106(H106), C111(H111), C112(H112),
 C113(H113), C114(H114), C119(H119), C120(H120), C121(H121), C122(H122),
 C127(H127), C128(H128), C129(H129), C130(H130)
3.b Idealised Me refined as rotating group:
 C206(H20A,H20B,H20C), C207(H20D,H20E,H20F), C208(H20G,H20H,H20I), C209(H20J,
 H20K,H20L), C210(H21A,H21B,H21C)
;
_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 1.090
_oxdiff_exptl_absorpt_empirical_full_min 0.954
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.435
_shelx_estimated_absorpt_t_max   0.845
_shelx_res_checksum              14728