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_7247036
_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_compound_source        no
_chemical_formula_moiety
'C48 H24 N8 Sn, C11 O11 Ir4, C20 H30 Cr, 2(C6 H4 Cl2)'
_chemical_formula_sum            'C91 H62 Cl4 Cr Ir4 N8 O11 Sn'
_chemical_formula_weight         2524.77
_chemical_melting_point          ?
_chemical_name_systematic
'Decamethylchromosenium salt of tin(II) naphthalocyanine coordinated Ir4(CO)11 cluster, dichlorobenzene solvate'
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2023-05-28 deposited with the CCDC.	2023-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                109.856(5)
_cell_angle_beta                 98.694(7)
_cell_angle_gamma                95.271(7)
_cell_formula_units_Z            4
_cell_length_a                   16.1813(18)
_cell_length_b                   14.7119(8)
_cell_length_c                   37.959(2)
_cell_measurement_reflns_used    3883
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.7070
_cell_measurement_theta_min      2.7300
_cell_volume                     8301.3(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    WinGx
_computing_publication_material  WinGx
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_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  0.1261
_diffrn_reflns_av_sigmaI/netI    0.4101
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            63204
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.758
_diffrn_reflns_theta_min         1.957
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.006
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.020
_exptl_crystal_description       needle
_exptl_crystal_F_000             4808
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: o-dichlorobenzene/n-hexane'
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.021
_refine_diff_density_max         8.541
_refine_diff_density_min         -4.495
_refine_diff_density_rms         0.498
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2088
_refine_ls_number_reflns         39142
_refine_ls_number_restraints     2985
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.2689
_refine_ls_R_factor_gt           0.1638
_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^)+(0.1768P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3552
_refine_ls_wR_factor_ref         0.3897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14121
_reflns_number_total             39142
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9577\% 
 around [0.99 0.10 0.12] (reciprocal) or [1.00 -0.00 -0.00] (direct)
;
_cod_data_source_file            d3ce00564j2.cif
_cod_data_source_block           DMCpCrIr4CO11SnNc2C6H4Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7247026--7247038.cif.
;
_cod_original_cell_volume        8301.4(12)
_cod_database_code               7247036
_shelx_estimated_absorpt_t_min   0.336
_shelx_estimated_absorpt_t_max   0.867
_oxdiff_twin_items               2
_oxdiff_twin_integration_method  simultaneous
_shelxl_version_number           2013-2
_shelx_res_checksum              39241