Self-assembly of [Sn(OPMe3)3(CF3SO3)2]6 metallocyclic Sn(ii) hexamer stacks with CF3-lined channel interiors
Cairns, Kelsey R.; King, Rhys P.; Levason, William; Reid, Gillian; CrystEngComm  (2022) –; doi:10.1039/D2CE01029A

data_7245358
_publ_section_title
;
 Self-assembly of [Sn(OPMe3)3(CF3SO3)2]6 metallocyclic Sn(ii) hexamer
 stacks with CF3-lined channel interiors
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01029A
_journal_year                    2022
_chemical_formula_moiety         'C9 H27 O3 P3 Sn, 2(C F3 O3 S), 0.167[C6H14]'
_chemical_formula_sum            'C12 H29.33 F6 O9 P3 S2 Sn'
_chemical_formula_weight         707.40
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-11 deposited with the CCDC.	2022-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   24.5947(4)
_cell_length_b                   24.5947(4)
_cell_length_c                   7.88970(10)
_cell_measurement_reflns_used    19430
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.7370
_cell_measurement_theta_min      1.8870
_cell_volume                     4133.08(11)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            23416
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.996
_diffrn_reflns_theta_min         2.753
_exptl_absorpt_coefficient_mu    1.330
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       block
_exptl_crystal_F_000             2126
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         6587
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0193
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+1.9847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6029
_reflns_number_total             6587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01029a2.cif
_cod_data_source_block           krc094b_1
_cod_original_cell_volume        4133.08(14)
_cod_database_code               7245358
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.825
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P3-C8 \\sim P3-C8B
 with sigma of 0.02
 P3-C7 \\sim P3-C7B
 with sigma of 0.02
 P3-C9 \\sim P3-C9B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C9B)
Uanis(C7) = Uanis(C7B)
Uanis(C8) = Uanis(C8B)
4. Others
 Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=
 Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
5.a Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C),
 C7B(H7BA,H7BB,H7BC), C9B(H9BA,H9BB,H9BC), C8B(H8BA,H8BB,H8BC)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 50 electrons were 
found in a volume of 272\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.167[C6H14] per Asymmetric Unit 
which account for 50 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              52374
_shelx_fab_checksum              95666
_olex2_submission_special_instructions 'No special instructions were received'