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_7709204
_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
'C18 H36 Cs N2 O6, C74 H32 N16 O10 Ru3 Sn2, C18 H36 K N2 O6, 3(C6 H4 Cl2), 1[C6H4Cl2]'
_chemical_formula_sum            'C134 H120 Cl8 Cs K N20 O22 Ru3 Sn2'
_chemical_formula_weight         3358.69
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-14
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.2701(4)
_cell_length_b                   22.9467(5)
_cell_length_c                   22.6093(3)
_cell_measurement_reflns_used    34677
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      28.5340
_cell_measurement_theta_min      1.7800
_cell_volume                     13629.2(4)
_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-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (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      101(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.918
_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    -47.00 -20.00   1.00   80.00    --  -12.05 -57.00 150.00   27
  2  \w    -23.00   3.00   1.00   80.00    --  -12.05 -57.00-180.00   26
  3  \w    -63.00   3.00   1.00   80.00    --  -12.05 -57.00 -60.00   66
  4  \w    -62.00  33.00   1.00   80.00    --   12.05 -57.00  60.00   95
  5  \w    -13.00  76.00   1.00   80.00    --   12.05  57.00-150.00   89
  6  \w     60.00  85.00   1.00   80.00    --   12.05  19.00  30.00   25
  7  \w    -26.00 -24.00   1.00   80.00    --   12.05  19.00  30.00    2
;
_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      -0.0251742000
_diffrn_orient_matrix_UB_12      0.0111285000
_diffrn_orient_matrix_UB_13      0.0012515000
_diffrn_orient_matrix_UB_21      -0.0085020000
_diffrn_orient_matrix_UB_22      -0.0232190000
_diffrn_orient_matrix_UB_23      -0.0181958000
_diffrn_orient_matrix_UB_31      -0.0048221000
_diffrn_orient_matrix_UB_32      -0.0170985000
_diffrn_orient_matrix_UB_33      0.0255225000
_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  0.0647
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            121049
_diffrn_reflns_point_group_measured_fraction_full 0.916
_diffrn_reflns_point_group_measured_fraction_max 0.776
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.662
_diffrn_reflns_theta_min         1.775
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84390
_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    1.637
_exptl_crystal_description       plate
_exptl_crystal_F_000             6728
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.108
_refine_diff_density_max         5.378
_refine_diff_density_min         -3.666
_refine_diff_density_rms         0.243
_refine_ls_abs_structure_details
;
 Flack x determined using 7674 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1576
_refine_ls_number_reflns         29927
_refine_ls_number_restraints     1575
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0882
_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^)+(0.1475P)^2^+89.8991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2455
_reflns_Friedel_coverage         0.652
_reflns_Friedel_fraction_full    0.828
_reflns_Friedel_fraction_max     0.627
_reflns_number_gt                22777
_reflns_number_total             29927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04061h2.cif
_cod_data_source_block           exp_2344_int1
_cod_database_code               7709204
_chemical_oxdiff_formula         'C32 H16 Ru3 O16 Cs3 Cl4'
_shelx_shelxl_version_number     2018/3
_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 1.279
_oxdiff_exptl_absorpt_empirical_full_min 0.848
_smtbx_masks_special_details
;
A solvent mask was calculated and 340 electrons were 
found in a volume of 1388\%A^3^ in 5 voids per unit cell. 
This is consistent with the presence of 
1[C6H4Cl2] per Asymmetric Unit 
which account for 296 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_estimated_absorpt_t_min   0.591
_shelx_estimated_absorpt_t_max   0.880
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O306-C306 \\sim O310-C310 \\sim O303-C303 \\sim O308-C308 \\sim O309-C309
\\sim O307-C307 \\sim O305-
 C305 \\sim O302-C302 \\sim O301-C301 \\sim O304-C304
 with sigma of 0.02
 Ru32-C306 \\sim Ru33-C310 \\sim Ru31-C303 \\sim Ru33-C309 \\sim Ru33-C308
\\sim Ru32-C305 \\sim Ru33-
 C307 \\sim Ru31-C301 \\sim Ru31-C302 \\sim Ru32-C304
 with sigma of 0.02
 Sn21-Ru31 \\sim Sn11-Ru32
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C71) \\sim Ueq,
Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C82) \\sim Ueq,
Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86)
\\sim Ueq, 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(C212) \\sim Ueq, Uanis(C213) \\sim Ueq,
Uanis(C214) \\sim Ueq, Uanis(C215) \\sim Ueq, Uanis(C216) \\sim Ueq,
Uanis(C217) \\sim Ueq, Uanis(C218) \\sim Ueq, Uanis(C219) \\sim Ueq,
Uanis(C220) \\sim Ueq, Uanis(C221) \\sim Ueq, Uanis(C222) \\sim Ueq,
Uanis(C223) \\sim Ueq, Uanis(C224) \\sim Ueq, Uanis(C225) \\sim Ueq,
Uanis(C226) \\sim Ueq, Uanis(C227) \\sim Ueq, Uanis(C228) \\sim Ueq,
Uanis(C229) \\sim Ueq, Uanis(C230) \\sim Ueq, Uanis(C231) \\sim Ueq,
Uanis(C232) \\sim Ueq, Uanis(C301) \\sim Ueq, Uanis(C302) \\sim Ueq,
Uanis(C303) \\sim Ueq, Uanis(C304) \\sim Ueq, Uanis(C305) \\sim Ueq,
Uanis(C306) \\sim Ueq, Uanis(C307) \\sim Ueq, Uanis(C308) \\sim Ueq,
Uanis(C309) \\sim Ueq, Uanis(C310) \\sim Ueq, Uanis(C401) \\sim Ueq,
Uanis(C402) \\sim Ueq, Uanis(C403) \\sim Ueq, Uanis(C404) \\sim Ueq,
Uanis(C405) \\sim Ueq, Uanis(C406) \\sim Ueq, Uanis(C407) \\sim Ueq,
Uanis(C408) \\sim Ueq, Uanis(C409) \\sim Ueq, Uanis(C410) \\sim Ueq,
Uanis(C411) \\sim Ueq, Uanis(C412) \\sim Ueq, Uanis(C413) \\sim Ueq,
Uanis(C414) \\sim Ueq, Uanis(C415) \\sim Ueq, Uanis(C416) \\sim Ueq,
Uanis(C417) \\sim Ueq, Uanis(C418) \\sim Ueq, Uanis(C501) \\sim Ueq,
Uanis(C502) \\sim Ueq, Uanis(C503) \\sim Ueq, Uanis(C504) \\sim Ueq,
Uanis(C505) \\sim Ueq, Uanis(C506) \\sim Ueq, Uanis(C507) \\sim Ueq,
Uanis(C508) \\sim Ueq, Uanis(C509) \\sim Ueq, Uanis(C510) \\sim Ueq,
Uanis(C511) \\sim Ueq, Uanis(C512) \\sim Ueq, Uanis(C513) \\sim Ueq,
Uanis(C514) \\sim Ueq, Uanis(C515) \\sim Ueq, Uanis(C516) \\sim Ueq,
Uanis(C517) \\sim Ueq, Uanis(C518) \\sim Ueq, 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, Uanis(N201) \\sim Ueq, Uanis(N202) \\sim Ueq,
Uanis(N203) \\sim Ueq, Uanis(N204) \\sim Ueq, Uanis(N205) \\sim Ueq,
Uanis(N206) \\sim Ueq, Uanis(N207) \\sim Ueq, Uanis(N208) \\sim Ueq,
Uanis(N401) \\sim Ueq, Uanis(N402) \\sim Ueq, Uanis(N501) \\sim Ueq,
Uanis(N502) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C306) \\sim Ueq, Uanis(C305) \\sim Ueq, Uanis(C304) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(C304) = Uanis(C301)
Uanis(C303) = Uanis(C306)
Uanis(C305) = Uanis(C302)
5.a Free rotating group:
 Cl61(Cl62,C61,C62,C63,C64,C65,C66), Cl72(Cl71,C71,C72,C73,C74,C75,C76),
 Cl82(Cl81,C81,C82,C83,C84,C85,C86)
5.b Secondary CH2 refined with riding coordinates:
 C401(H40A,H40B), C402(H40C,H40D), C403(H40E,H40F), C404(H40G,H40H), C405(H40I,
 H40J), C406(H40K,H40L), C407(H40M,H40N), C408(H40O,H40P), C409(H40Q,H40R),
 C410(H41A,H41B), C411(H41C,H41D), C412(H41E,H41F), C413(H41G,H41H), C414(H41I,
 H41J), C415(H41K,H41L), C416(H41M,H41N), C417(H41O,H41P), C418(H41Q,H41R),
 C501(H50A,H50B), C502(H50C,H50D), C503(H50E,H50F), C504(H50G,H50H), C505(H50I,
 H50J), C506(H50K,H50L), C507(H50M,H50N), C508(H50O,H50P), C509(H50Q,H50R),
 C510(H51A,H51B), C511(H51C,H51D), C512(H51E,H51F), C513(H51G,H51H), C514(H51I,
 H51J), C515(H51K,H51L), C516(H51M,H51N), C517(H51O,H51P), C518(H51Q,H51R)
5.c Aromatic/amide H refined with riding coordinates:
 C63(H63), C64(H64), C65(H65), C66(H66), C73(H73), C74(H74), C75(H75),
 C76(H76), C83(H83), C84(H84), C85(H85), C86(H86), 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), C203(H203), C204(H204), C205(H205), C206(H206),
 C211(H211), C212(H212), C213(H213), C214(H214), C219(H219), C220(H220),
 C221(H221), C222(H222), C227(H227), C228(H228), C229(H229), C230(H230)
;
_shelx_res_checksum              2050
_shelx_hkl_checksum              18618
_shelx_fab_checksum              9002