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_4346668
_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
'(C42 H31 Sn Rh Cl2), (C18 H36 O6 N2 Na), (C6 H4 Cl2)'
_chemical_formula_sum            'C66 H71 Cl4 N10 Na O6 Rh Sn'
_chemical_formula_weight         1486.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.741(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0896(1)
_cell_length_b                   26.0217(3)
_cell_length_c                   18.9023(2)
_cell_measurement_reflns_used    22340
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     6406.09(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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      180(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 0.887
_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  0.0407
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            57412
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.815
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.371
_diffrn_reflns_theta_min         1.811
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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    1.542
_exptl_crystal_description       plate
_exptl_crystal_F_000             3036
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 9132 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.009(8)
_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     1579
_refine_ls_number_reflns         28726
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0247P)^2^+10.4999P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    0.897
_reflns_Friedel_fraction_max     0.739
_reflns_number_gt                23680
_reflns_number_total             28726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01906_si_002.cif
_cod_data_source_block           PMCpRhCl2SnPc_cryptNa_C6H4Cl2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4346668
_shelx_estimated_absorpt_t_min   0.730
_shelx_estimated_absorpt_t_max   0.971
_shelxl_version_number           2013-2
_shelx_res_checksum              46374
_shelx_hkl_checksum              48587