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_7245357
_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         'C10 H27 F3 O6 P3 Pb S, C F3 O3 S'
_chemical_formula_sum            'C11 H27 F6 O9 P3 Pb S2'
_chemical_formula_weight         781.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-19
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6427)
;
_audit_update_record
;
2022-04-29 deposited with the CCDC.	2022-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.257(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7633(3)
_cell_length_b                   14.2131(4)
_cell_length_c                   18.8859(5)
_cell_measurement_reflns_used    22183
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      31.7630
_cell_measurement_theta_min      1.8170
_cell_volume                     2593.57(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -45.00 -16.00   0.50    0.30    --   21.25 -19.00 -60.00   58
  2  \w    -66.00 -16.00   0.50    0.30    --   21.25 -19.00 -90.00  100
  3  \w    -62.00 -18.00   0.50    0.30    --   21.25 -19.00  60.00   88
  4  \w    -18.00  23.00   0.50    0.30    --   21.25 -77.00 120.00   82
  5  \w     22.00  64.00   0.50    0.30    --  -18.75  19.00  60.00   84
  6  \w    -73.00  -6.00   0.50    0.30    --  -18.75 118.00 116.00  134
  7  \w     22.00  64.00   0.50    0.30    --  -18.75  19.00   0.00   84
  8  \w     12.00  76.00   0.50    0.30    --   21.25-118.00  30.00  128
  9  \w      0.00  65.00   0.50    0.30    --   21.25 -99.00  60.00  130
 10  \w     22.00  64.00   0.50    0.30    --  -18.75  19.00-150.00   84
 11  \w     22.00  64.00   0.50    0.30    --  -18.75  19.00-180.00   84
 12  \w    -56.00   9.00   0.50    0.30    --  -18.75 -57.00-180.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0020691000
_diffrn_orient_matrix_UB_12      0.0138502000
_diffrn_orient_matrix_UB_13      0.0359100000
_diffrn_orient_matrix_UB_21      -0.0104961000
_diffrn_orient_matrix_UB_22      0.0473979000
_diffrn_orient_matrix_UB_23      -0.0112821000
_diffrn_orient_matrix_UB_31      -0.0726179000
_diffrn_orient_matrix_UB_32      -0.0071898000
_diffrn_orient_matrix_UB_33      -0.0049162000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30244
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.108
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.931
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
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    2.002
_exptl_crystal_description       prism
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.716
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0223
_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^)+(0.0160P)^2^+0.9794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5816
_reflns_number_total             6662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01029a2.cif
_cod_data_source_block           krc121a_1
_cod_database_code               7245357
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         PbS2O9F6P3C11H27
_chemical_oxdiff_usercomment     467a
_shelx_estimated_absorpt_t_max   0.544
_shelx_estimated_absorpt_t_min   0.168
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C2(H2A,
 H2B,H2C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              60269
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.966
_oxdiff_exptl_absorpt_empirical_full_min 0.644