Complexes of transition metal carbonyl clusters with tin(II) phthalocyanine in neutral and radical anion states: methods of synthesis, structures and properties
Romanenko, Nikita R.; Kuzmin, Alexey V.; Khasanov, Salavat S.; Faraonov, Maxim A.; Yudanova, Evgeniya I.; Nakano, Yoshiaki; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Konarev, Dmitri V.; Dalton Transactions  (2022) –; doi:10.1039/D1DT04061H

data_7709200
_publ_section_title
;
 Complexes of transition metal carbonyl clusters with tin(II)
 phthalocyanine in neutral and radical anion states: methods of synthesis,
 structures and properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04061H
_journal_year                    2022
_chemical_formula_moiety         'C43 H16 Ir4 N8 O11 Sn, C10 H15 Cr0.5'
_chemical_formula_sum            'C53 H31 Cr0.5 Ir4 N8 O11 Sn'
_chemical_formula_weight         1869.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-10
_audit_creation_method
;
FinalCif V89 by Daniel Kratzert, Freiburg 2021,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2021-10-14 deposited with the CCDC.	2021-12-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.584(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.9498(5)
_cell_length_b                   15.1713(2)
_cell_length_c                   14.5364(4)
_cell_measurement_reflns_used    11988
_cell_measurement_temperature    129.9(6)
_cell_measurement_theta_max      32.6670
_cell_measurement_theta_min      2.1830
_cell_volume                     5235.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_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      129.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.913
_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  49.00   1.00   80.00    --   20.30 -57.00 -30.00  102
  2  \w     -2.00  90.00   1.00   80.00    --   20.30  57.00 120.00   92
  3  \w    -70.00   6.00   1.00   80.00    --  -20.45 -57.00-150.00   76
  4  \w    -39.00  49.00   1.00   80.00    --  -20.45  19.00-120.00   88
  5  \w    -17.00  17.00   1.00   80.00    --  -20.45 -99.00 120.00   34
;
_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      0.0010140000
_diffrn_orient_matrix_UB_12      0.0338122000
_diffrn_orient_matrix_UB_13      -0.0333758000
_diffrn_orient_matrix_UB_21      0.0096333000
_diffrn_orient_matrix_UB_22      0.0301931000
_diffrn_orient_matrix_UB_23      0.0359011000
_diffrn_orient_matrix_UB_31      0.0282769000
_diffrn_orient_matrix_UB_32      -0.0114773000
_diffrn_orient_matrix_UB_33      -0.0041675000
_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  0.0543
_diffrn_reflns_av_unetI/netI     0.0945
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31472
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.907
_diffrn_reflns_theta_min         1.716
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
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    2.372
_exptl_crystal_description       block
_exptl_crystal_F_000             3452
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.056
_refine_diff_density_max         5.304
_refine_diff_density_min         -2.909
_refine_diff_density_rms         0.323
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.277(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         16896
_refine_ls_number_restraints     367
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0494P)^2^+22.8678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1376
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.807
_reflns_number_gt                14494
_reflns_number_total             16896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04061h2.cif
_cod_data_source_block           exp_1146_int3
_cod_original_formula_sum        'C53 H31 Cr0.50 Ir4 N8 O11 Sn'
_cod_database_code               7709200
_chemical_oxdiff_formula         'Ir3 Cr1 C36 H60 O16'
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.723(11)
 0.277(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq,
Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C106) \\sim Ueq,
Uanis(C107) \\sim Ueq, Uanis(C108) \\sim Ueq, Uanis(C109) \\sim Ueq,
Uanis(C110) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(C112) \\sim Ueq,
Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(C115) \\sim Ueq,
Uanis(C116) \\sim Ueq, Uanis(C117) \\sim Ueq, Uanis(C118) \\sim Ueq,
Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(C121) \\sim Ueq,
Uanis(C122) \\sim Ueq, Uanis(C123) \\sim Ueq, Uanis(C124) \\sim Ueq,
Uanis(C125) \\sim Ueq, Uanis(C126) \\sim Ueq, Uanis(C127) \\sim Ueq,
Uanis(C128) \\sim Ueq, Uanis(C129) \\sim Ueq, Uanis(C130) \\sim Ueq,
Uanis(C131) \\sim Ueq, Uanis(C132) \\sim Ueq, Uanis(C201) \\sim Ueq,
Uanis(C202) \\sim Ueq, Uanis(C203) \\sim Ueq, Uanis(C204) \\sim Ueq,
Uanis(C205) \\sim Ueq, Uanis(C206) \\sim Ueq, Uanis(C207) \\sim Ueq,
Uanis(C208) \\sim Ueq, Uanis(C209) \\sim Ueq, Uanis(C210) \\sim Ueq,
Uanis(C211) \\sim Ueq, Uanis(C311) \\sim Ueq, Uanis(C312) \\sim Ueq,
Uanis(C313) \\sim Ueq, Uanis(C314) \\sim Ueq, Uanis(C315) \\sim Ueq,
Uanis(C316) \\sim Ueq, Uanis(C317) \\sim Ueq, Uanis(C318) \\sim Ueq,
Uanis(C319) \\sim Ueq, Uanis(C320) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N101) \\sim Ueq, Uanis(N102) \\sim Ueq, Uanis(N103) \\sim Ueq,
Uanis(N104) \\sim Ueq, Uanis(N105) \\sim Ueq, Uanis(N106) \\sim Ueq,
Uanis(N107) \\sim Ueq, Uanis(N108) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4.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)
4.b Idealised Me refined as rotating group:
 C316(H31A,H31B,H31C), C317(H31D,H31E,H31F), C318(H31G,H31H,H31I), C319(H31J,
 H31K,H31L), C320(H32A,H32B,H32C)
;
_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 2.736
_oxdiff_exptl_absorpt_empirical_full_min 0.722
_shelx_res_checksum              1939
_shelx_hkl_checksum              26632