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_7709202
_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
'C42 H16 Cl N8 O10 Os3 Sn, C20 H30 Cr, C6 H4 Cl2'
_chemical_formula_sum            'C68 H50 Cl3 Cr N8 O10 Os3 Sn'
_chemical_formula_weight         1986.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 96.102(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8961(4)
_cell_length_b                   20.0969(4)
_cell_length_c                   19.6999(4)
_cell_measurement_reflns_used    40850
_cell_measurement_temperature    130(4)
_cell_measurement_theta_max      32.4020
_cell_measurement_theta_min      2.2680
_cell_volume                     6651.4(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      130(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     -8.00  94.00   0.50   40.00    --   20.30  57.00 -30.00  204
  2  \w    -13.00  99.00   0.50   40.00    --   20.30  77.00  90.00  224
  3  \w      1.00  81.00   0.50   40.00    --   20.30-130.00  97.45  160
  4  \w    -55.00  45.00   0.50   40.00    --   20.30 -37.00-180.00  200
  5  \w     35.00  80.00   0.50   40.00    --   20.30 178.00-150.00   90
  6  \w    -25.00  62.00   0.50   40.00    --   20.30 -99.00 -30.00  174
  7  \w     -1.00  96.00   0.50   40.00    --   20.30  37.00-120.00  194
  8  \w    -95.00 -43.00   0.50   40.00    --  -20.45 151.00  90.37  104
  9  \w    -21.00  17.00   0.50   40.00    --  -20.45 -99.00-180.00   76
;
_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      -0.0259631000
_diffrn_orient_matrix_UB_12      0.0146070000
_diffrn_orient_matrix_UB_13      -0.0265323000
_diffrn_orient_matrix_UB_21      -0.0257883000
_diffrn_orient_matrix_UB_22      0.0101551000
_diffrn_orient_matrix_UB_23      0.0242215000
_diffrn_orient_matrix_UB_31      0.0210345000
_diffrn_orient_matrix_UB_32      0.0304856000
_diffrn_orient_matrix_UB_33      0.0046406000
_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  0.0420
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            90186
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.679
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.424
_exptl_absorpt_correction_T_max  0.453
_exptl_absorpt_correction_T_min  0.187
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
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            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_description       block
_exptl_crystal_F_000             3788
_exptl_crystal_size_max          0.512
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.166
_refine_diff_density_max         5.793
_refine_diff_density_min         -2.337
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         13587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0499P)^2^+64.0938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12022
_reflns_number_total             13587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04061h2.cif
_cod_data_source_block           exp_1131_int1
_cod_database_code               7709202
_chemical_oxdiff_formula         C68H50Cl3CrN8O10Os3Sn
_shelx_shelxl_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   13418
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.834
_shelx_estimated_absorpt_t_min   0.138
_shelx_estimated_absorpt_t_max   0.415
_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
Uanis(Os1A) = Uanis(Os1B)
Uanis(Os2A) = Uanis(Os2B)
Uanis(Cl2A) = Uanis(Cl2B)
Uanis(O24A) = Uanis(O24B)
Uanis(O25A) = Uanis(O25B)
Uanis(O26A) = Uanis(O26B)
Uanis(O27A) = Uanis(O27B)
Uanis(O28A) = Uanis(O28B)
Uanis(O29A) = Uanis(O29B)
Uanis(O20A) = Uanis(O20B)
Uanis(C24A) = Uanis(C24B)
Uanis(C25A) = Uanis(C25B)
Uanis(C26A) = Uanis(C26B)
Uanis(C27A) = Uanis(C27B)
Uanis(C28A) = Uanis(C28B)
Uanis(C29A) = Uanis(C29B)
Uanis(C21A) = Uanis(C21B)
3. Others
 Sof(Os1B)=Sof(Os2B)=Sof(Cl2B)=Sof(O24B)=Sof(O25B)=Sof(O26B)=Sof(O27B)=
 Sof(O28B)=Sof(O29B)=Sof(O20B)=Sof(C24B)=Sof(C25B)=Sof(C26B)=Sof(C27B)=
 Sof(C28B)=Sof(C29B)=Sof(C21B)=1-FVAR(1)
 Sof(Os1A)=Sof(Os2A)=Sof(Cl2A)=Sof(O24A)=Sof(O25A)=Sof(O26A)=Sof(O27A)=
 Sof(O28A)=Sof(O29A)=Sof(O20A)=Sof(C24A)=Sof(C25A)=Sof(C26A)=Sof(C27A)=
 Sof(C28A)=Sof(C29A)=Sof(C21A)=FVAR(1)
4.a Free rotating group:
 Os1A(Os2A,Cl2A,O24A,O25A,O26A,O27A,O28A,O29A,O20A,C24A,C25A,C26A,C27A,C28A,
 C29A,C21A), Os1B(Os2B,Cl2B,O24B,O25B,O26B,O27B,O28B,O29B,O20B,C24B,C25B,C26B,
 C27B,C28B,C29B,C21B)
4.b 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), C403(H403), C404(H404),
 C405(H405), C406(H406)
4.c Idealised Me refined as rotating group:
 C306(H30A,H30B,H30C), C307(H30D,H30E,H30F), C308(H30G,H30H,H30I), C309(H30J,
 H30K,H30L), C310(H31A,H31B,H31C), C316(H31D,H31E,H31F), C317(H31G,H31H,H31I),
 C318(H31J,H31K,H31L), C319(H31M,H31N,H31O), C320(H32A,H32B,H32C)
;
_shelx_res_checksum              1818
_shelx_hkl_checksum              384