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_4317734
_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            'C48 H56 N24 O8 Sn7'
_chemical_formula_weight         1928.00
_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
_cell_angle_alpha                86.620(10)
_cell_angle_beta                 84.690(10)
_cell_angle_gamma                80.740(10)
_cell_formula_units_Z            1
_cell_length_a                   11.483(2)
_cell_length_b                   11.773(2)
_cell_length_c                   12.155(2)
_cell_measurement_temperature    180(2)
_cell_volume                     1613.2(5)
_computing_cell_refinement       maXus
_computing_data_collection       maXus
_computing_data_reduction        maXus
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    teXsan
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_sigmaI/netI    0.0970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10454
_diffrn_reflns_theta_max         22.63
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    2.733
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  1.021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

multi-scan from symmetry-related measurements (Blessing 1995)
;
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_F_000             926
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.600
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.017
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_obs          0.0521
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+13.3316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1350
_refine_ls_wR_factor_obs         0.1113
_reflns_number_observed          3030
_reflns_number_total             4176
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011090r_2.cif
_cod_data_source_block           dw0022
_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.

'_exptl_absorpt_correction_type' value 'multiscan'
changed to 'multi-scan' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+13.3316P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+13.3316P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4317734