Formation of Double Cubanes [Sn7(NR)8] in the Reactions of Pyridyl and Pyrimidinyl Amines with Sn(NMe2)2: A Synthetic and Theoretical Study
David R. Armstrong; Francesca Benevelli; Andrew D. Bond; Neil Feeder; Eilis A. Harron; Alexander D. Hopkins; Mary McPartlin; David Moncrieff; David Sáez; Elsje A. Quadrelli; Anthony D. Woods; Dominic S. Wright; Inorganic Chemistry 41 (2002) 1492–1501; doi:10.1021/ic011090r

data_4317735
_publ_section_title
;
 Formation of Double Cubanes [Sn7(NR)8] in the Reactions of Pyridyl and
 Pyrimidinyl Amines with Sn(NMe2)2: A Synthetic and Theoretical Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1492
_journal_page_last               1501
_journal_paper_doi               10.1021/ic011090r
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C56 H72 N24 O2 Sn7'
_chemical_formula_weight         1944.21
_chemical_name_systematic
;

  ?

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.066(2)
_cell_angle_beta                 81.957(3)
_cell_angle_gamma                75.450(3)
_cell_formula_units_Z            1
_cell_length_a                   12.1860(4)
_cell_length_b                   12.7060(8)
_cell_length_c                   12.9930(8)
_cell_measurement_reflns_used    11614
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.91
_cell_volume                     1920.40(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
;

  ?

;
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9706
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    2.291
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.693
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+6.8766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1402
_reflns_number_gt                5001
_reflns_number_total             6762
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011090r_3.cif
_cod_data_source_block           dw9946
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317735