Assembly of High-Nuclearity Sn26, Sn34-Oxo Clusters: Solvent Strategy and Inorganic Sn Incorporation
Zhu, Yu; Zhang, Lei; Zhang, Jian; Chemical Science  (2019) –; doi:10.1039/C9SC02503K

data_1552184
_publ_section_title
;
 Assembly of High-Nuclearity Sn26, Sn34-Oxo Clusters: Solvent Strategy and
 Inorganic Sn Incorporation
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02503K
_journal_year                    2019
_chemical_formula_sum            'C78 H188 O52 Sn12'
_chemical_formula_weight         3382.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-08-01 deposited with the CCDC.    2019-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.285(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.8261(15)
_cell_length_b                   20.7264(8)
_cell_length_c                   19.1980(15)
_cell_measurement_reflns_used    6994
_cell_measurement_temperature    100.02(13)
_cell_measurement_theta_max      74.5530
_cell_measurement_theta_min      4.4530
_cell_volume                     6413.5(9)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100.02(13)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19839
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        62.492
_diffrn_reflns_theta_max         62.492
_diffrn_reflns_theta_min         3.474
_exptl_absorpt_coefficient_mu    18.902
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         3.068
_refine_diff_density_min         -1.533
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         9846
_refine_ls_number_restraints     340
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1412
_refine_ls_R_factor_gt           0.0997
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+400.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1984
_refine_ls_wR_factor_ref         0.2143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6878
_reflns_number_total             9846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02503k2.cif
_cod_data_source_block           x_sq_CCDC2
_cod_database_code               1552184
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              76624
_shelx_fab_checksum              81122