Heterotrimetallic paramagnetic complex of ring reduced tin(ii) hexadecachlorophthalocyanine
Romanenko, Nikita R.; Faraonov, Maxim A.; Osipov, Nikita G.; Kuzmin, Alexey V.; Khasanov, Salavat S.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Konarev, Dmitri V.; New Journal of Chemistry 47 (2023) 6924–6931; doi:10.1039/D3NJ00506B

data_7062380
_publ_section_title
;
 Heterotrimetallic paramagnetic complex of ring reduced tin(ii)
 hexadecachlorophthalocyanine
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6924
_journal_page_last               6931
_journal_paper_doi               10.1039/D3NJ00506B
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety
'2(C6 H4 Cl2), 2(C18 H36 K N2 O6), C32 Cl18 N8 Sn'
_chemical_formula_sum            'C80 H80 Cl22 K2 N12 O12 Sn'
_chemical_formula_weight         2378.35
_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     direct
_audit_creation_date             2022-10-26
_audit_creation_method
;FinalCif V113 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2022-10-26 deposited with the CCDC.	2023-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                93.386(2)
_cell_angle_beta                 97.165(2)
_cell_angle_gamma                98.588(2)
_cell_formula_units_Z            2
_cell_length_a                   14.6176(3)
_cell_length_b                   16.7506(3)
_cell_length_c                   19.9647(4)
_cell_measurement_reflns_used    21629
_cell_measurement_temperature    101(1)
_cell_measurement_theta_max      29.2950
_cell_measurement_theta_min      2.3250
_cell_volume                     4780.81(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_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      101.15
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.833
_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    -62.00  41.00   1.00   55.00    --   11.89 -57.00  60.00  103
  2  \w      3.00  63.00   1.00   55.00    --   11.89  48.00 -29.00   60
  3  \w    -12.00  76.00   1.00   55.00    --   11.89  57.00-150.00   88
  4  \w    -74.00   1.00   1.00   55.00    --  -12.05 -57.00 -60.00   75
  5  \w    -30.00  -5.00   1.00   55.00    --  -12.05 -57.00-180.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46711
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.523
_diffrn_reflns_theta_min         1.640
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.60a (Rigaku Oxford Diffraction, 2022)
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    1.652
_exptl_crystal_description       block
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1162
_refine_ls_number_reflns         22237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+1.5500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18160
_reflns_number_total             22237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00506b2.cif
_cod_data_source_block           exp_2390_int1
_cod_depositor_comments
'Adding full bibliography for 7062380--7062381.cif.'
_cod_database_code               7062380
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C105(H10I,
 H10J), C106(H10K,H10L), C107(H10M,H10N), C108(H10O,H10P), C109(H10Q,H10R),
 C110(H11A,H11B), C111(H11C,H11D), C112(H11E,H11F), C113(H11G,H11H), C114(H11I,
 H11J), C115(H11K,H11L), C116(H11M,H11N), C117(H11O,H11P), C118(H11Q,H11R),
 C201(H20A,H20B), C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H), C205(H20I,
 H20J), C206(H20K,H20L), C207(H20M,H20N), C208(H20O,H20P), C209(H20Q,H20R),
 C210(H21A,H21B), C211(H21C,H21D), C212(H21E,H21F), C213(H21G,H21H), C214(H21I,
 H21J), C215(H21K,H21L), C216(H21M,H21N), C217(H21O,H21P), C218(H21Q,H21R)
2.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C44(H44), C45(H45), C46(H46), C53(H53), C54(H54), C55(H55), C56(H56)
;
_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
;
_shelx_estimated_absorpt_t_min   0.600
_shelx_estimated_absorpt_t_max   0.922
_shelx_res_checksum              51218
_shelx_hkl_checksum              3721