Coordination Complexes of Transition Metals (M = Mo, Fe, Rh, and Ru) with Tin(II) Phthalocyanine in Neutral, Monoanionic, and Dianionic States.
Konarev, Dmitri V.; Kuzmin, Alexey V.; Nakano, Yoshiaki; Faraonov, Maxim A.; Khasanov, Salavat S.; Otsuka, Akihiro; Yamochi, Hideki; Saito, Gunzi; Lyubovskaya, Rimma N.; Inorganic chemistry 55 (2016) 1390–1402; doi:10.1021/acs.inorgchem.5b01906

data_4346667
_publ_section_title
;
 Coordination Complexes of Transition Metals (M = Mo, Fe, Rh, and Ru) with
 Tin(II) Phthalocyanine in Neutral, Monoanionic, and Dianionic States.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1390
_journal_page_last               1402
_journal_paper_doi               10.1021/acs.inorgchem.5b01906
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'(C71 H37 N16 Sn2 Mo o2), (C18 H36 N2 O6 Na) 3.5(C6 H4 Cl2)'
_chemical_formula_sum            'C110 H87 Cl7 Mo N18 Na O8 Sn2'
_chemical_formula_weight         2393.43
_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
_cell_angle_alpha                85.695(2)
_cell_angle_beta                 88.189(2)
_cell_angle_gamma                77.512(2)
_cell_formula_units_Z            2
_cell_length_a                   17.0023(4)
_cell_length_b                   17.4314(5)
_cell_length_c                   17.7859(3)
_cell_measurement_reflns_used    13250
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     5131.4(2)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_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 0.858
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_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  0.0331
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44402
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.048
_diffrn_reflns_theta_min         1.667
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            black
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       block
_exptl_crystal_F_000             2418
_exptl_crystal_size_max          0.455
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.116
_refine_diff_density_max         1.607
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1589
_refine_ls_number_reflns         23517
_refine_ls_number_restraints     1039
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+12.4907P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14971
_reflns_number_total             23517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01906_si_002.cif
_cod_data_source_block           CpMo(CO)2SnPc2_crypt(Na)_3.5C6H4Cl2
_cod_database_code               4346667
_shelx_estimated_absorpt_t_min   0.696
_shelx_estimated_absorpt_t_max   0.907
_shelxl_version_number           2013-2
_shelx_res_checksum              40377
_shelx_hkl_checksum              46010