Bis(μ2-4-nitrophenolato)bis(4-nitrophenolato)di-μ3-oxido-octaphenyltetratin chloroform sesquisolvate [+ solvate]: a tetranuclear stannoxane
Butler, Patrick; IUCrData 4 (2019) x191067–; doi:10.1107/S2414314619010678

data_1552164
_publ_section_title
;
 Bis(\m2-4-nitrophenolato)bis(4-nitrophenolato)di-\m3-oxido-octaphenyltetratin
 chloroform sesquisolvate [+ solvate]: a tetranuclear stannoxane
;
_journal_issue                   8
_journal_name_full               IUCrData
_journal_page_first              x191067
_journal_paper_doi               10.1107/S2414314619010678
_journal_volume                  4
_journal_year                    2019
_chemical_formula_iupac
'[Sn4 (C6 H5)8 (C6 H4 N O3)4 O2], 1.5C H Cl3, solvent'
_chemical_formula_moiety
'C72 H56 N4 O14 Sn4, 1.5(C H Cl3), [+  solvent]'
_chemical_formula_sum            'C73.5 H57.5 Cl4.5 N4 O14 Sn4'
_chemical_formula_weight         1855.02
_chemical_name_systematic
'Bis(\m~2~-4-nitrophenolato)bis(4-nitrophenolato)di-\m~3~-oxido-octaphenyltetratin chloroform sesquisolvate [+ solvate]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                72.349(2)
_cell_angle_beta                 79.800(2)
_cell_angle_gamma                89.8270(10)
_cell_formula_units_Z            4
_cell_length_a                   12.8262(2)
_cell_length_b                   22.1075(4)
_cell_length_c                   28.9552(5)
_cell_measurement_reflns_used    18171
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      73.59
_cell_measurement_theta_min      4.18
_cell_volume                     7689.0(2)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009) and Mercury (Macrae <i>et
al.</i>,  2008
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            52013
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.056
_diffrn_reflns_theta_min         3.990
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    12.177
_exptl_absorpt_correction_T_max  0.6148
_exptl_absorpt_correction_T_min  0.5841
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       plate
_exptl_crystal_F_000             3660
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.019
_exptl_crystal_size_rad          0.034
_refine_diff_density_max         3.878
_refine_diff_density_min         -2.318
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1801
_refine_ls_number_reflns         30192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+23.2885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1746
_refine_ls_wR_factor_ref         0.1967
_reflns_number_gt                21951
_reflns_number_total             30192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su4174sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C73.50 H57.50 Cl4.50 N4 O14 Sn4'
_cod_database_code               1552164
_cod_database_fobs_code          1552164
_shelx_hkl_checksum              33834
_shelx_res_checksum              43172
_shelx_fab_checksum              64680