Coordination Chemistry of N-Heterocyclic Stannylenes: A Combined Synthetic and Mössbauer Spectroscopy Study
Stephen M. Mansell; Rolfe H. Herber; Israel Nowik; Douglas H. Ross; Christopher A. Russell; Duncan F. Wass; Inorganic Chemistry 50 (2011) 2252–2263; doi:10.1021/ic101920x

data_4324597
_publ_contact_author
; 
    Dr. Chris Russell 
    School of Chemistry
    University of Bristol
    Cantock's Close
    BS8 1TS Bristol
    UK
;
_publ_contact_author_email
;
Chris.Russell@bristol.ac.uk
;
_publ_contact_author_fax         '0117 9290509'
_publ_contact_author_phone       '0117 9287655'
_publ_section_title
;
 Coordination Chemistry of N-Heterocyclic Stannylenes: A Combined
 Synthetic and M\"ossbauer Spectroscopy Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2252
_journal_page_last               2263
_journal_paper_doi               10.1021/ic101920x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C60 H76 Fe2 N4 O8 Sn2'
_chemical_formula_sum            'C60 H76 Fe2 N4 O8 Sn2'
_chemical_formula_weight         1330.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.069(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4655(16)
_cell_length_b                   11.7855(13)
_cell_length_c                   19.163(2)
_cell_measurement_reflns_used    4273
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.417
_cell_measurement_theta_min      2.319
_cell_volume                     2973.9(6)
_computing_cell_refinement       'APEX-II and SAINT (Bruker, 2001)'
_computing_data_collection       'APEX-II (Bruker, 2004)'
_computing_data_reduction        'SAINT v7.51A (BRUKER)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa-APEX-II area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25856
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.364
_exptl_absorpt_correction_T_max  0.933912
_exptl_absorpt_correction_T_min  0.735777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2007/4
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         6822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+2.4534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                4755
_reflns_number_total             6822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101920x_si_001_2.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4324597