Alkyltin clusters: the less symmetric Keggin isomers.
Hutchison, Danielle C.; Stern, Rebecca D.; Olsen, Morgan R.; Zakharov, Lev N.; Persson, Kristin A.; Nyman, May; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9804–9813; doi:10.1039/c8dt01950a

data_7046927
_publ_section_title
;
 Alkyltin clusters: the less symmetric Keggin isomers.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9804
_journal_page_last               9813
_journal_paper_doi               10.1039/c8dt01950a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C64 H159 Na O29 Sn13'
_chemical_formula_weight         2958.86
_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-2014/7
_audit_update_record
;
2018-04-18 deposited with the CCDC.
2018-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.8910(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0683(8)
_cell_length_b                   18.8014(6)
_cell_length_c                   24.5975(7)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      53.57
_cell_measurement_theta_min      3.06
_cell_volume                     10177.1(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       '\f nad \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            74384
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        54.039
_diffrn_reflns_theta_max         54.039
_diffrn_reflns_theta_min         2.167
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    25.454
_exptl_absorpt_correction_T_max  0.7507
_exptl_absorpt_correction_T_min  0.4912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             5744
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         2.033
_refine_diff_density_min         -1.744
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         12160
_refine_ls_number_restraints     1548
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0857
_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^)+(0.0938P)^2^+309.6281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8057
_reflns_number_total             12160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01950a2.cif
_cod_data_source_block           cu_mayr220_0m
_cod_depositor_comments
'Adding full bibliography for 7046925--7046927.cif.'
_cod_database_code               7046927
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.125
_shelx_estimated_absorpt_t_max   0.208
_shelx_res_checksum              75891