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_7709205
_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 N8 O11 Ru3 Sn, C20 H30 Cr, C6 H4 Cl2'
_chemical_formula_sum            'C69 H50 Cl2 Cr N8 O11 Ru3 Sn'
_chemical_formula_weight         1711.97
_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                 94.8720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.78010(10)
_cell_length_b                   20.05930(10)
_cell_length_c                   19.76710(10)
_cell_measurement_reflns_used    68094
_cell_measurement_temperature    119.95(10)
_cell_measurement_theta_max      35.0940
_cell_measurement_theta_min      1.8400
_cell_volume                     6629.51(6)
_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      119.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4566
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.949
_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    -11.00  68.00   1.00   25.00    --   25.71 -99.00-120.00   79
  2  \w    -48.00  43.00   1.00   25.00    --   25.71 -57.00  30.00   91
  3  \w     -8.00  97.00   1.00   25.00    --   25.71  77.00 150.00  105
  4  \w     -4.00  94.00   1.00   25.00    --   25.71  57.00 -60.00   98
  5  \w     -8.00  98.00   1.00   25.00    --   25.71  77.00  30.00  106
  6  \w    -25.00  68.00   1.00   25.00    --   25.71 -99.00   0.00   93
  7  \w    -25.00  68.00   1.00   25.00    --   25.71 -99.00 150.00   93
  8  \w     -2.00  63.00   1.00   25.00    --  -26.02   0.00 -60.00   65
  9  \w    -99.00 -46.00   1.00   25.00    --  -26.02   0.00 -60.00   53
;
_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      -0.0063322000
_diffrn_orient_matrix_UB_12      0.0331640000
_diffrn_orient_matrix_UB_13      0.0107693000
_diffrn_orient_matrix_UB_21      -0.0410932000
_diffrn_orient_matrix_UB_22      -0.0071595000
_diffrn_orient_matrix_UB_23      0.0022128000
_diffrn_orient_matrix_UB_31      0.0084041000
_diffrn_orient_matrix_UB_32      -0.0099376000
_diffrn_orient_matrix_UB_33      0.0343039000
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            179021
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.250
_diffrn_reflns_theta_min         1.586
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.346
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88838
_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    1.715
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         28227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+3.7572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23076
_reflns_number_total             28227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04061h2.cif
_cod_data_source_block           exp_1134_int1
_cod_database_code               7709205
_chemical_oxdiff_formula         C312Cl8Cr4N4O40Ru12Sn4
_shelx_shelxl_version_number     2018/3
_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.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), C403(H403), C404(H404),
 C405(H405), C406(H406)
2.b 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)
;
_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 1.247
_oxdiff_exptl_absorpt_empirical_full_min 0.873
_shelx_estimated_absorpt_t_min   0.629
_shelx_estimated_absorpt_t_max   0.824
_shelx_res_checksum              18787
_shelx_hkl_checksum              54019