Bulk assembly of a 0D organic tin(ii)chloride hybrid with high anti-water stability.
Peng, Hui; Wang, Xinxin; Zhang, Zhenheng; Tian, Ye; Xiao, Yonghao; Hu, Jinming; Wang, Jianping; Zou, Bingsuo; Chemical communications (Cambridge, England) 57 (2021) 8162–8165; doi:10.1039/d1cc02814f

data_7128642
_publ_section_title
;
 Bulk assembly of a 0D organic tin(ii)chloride hybrid with high anti-water
 stability.
;
_journal_issue                   66
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8162
_journal_page_last               8165
_journal_paper_doi               10.1039/d1cc02814f
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'Cl3 Sn, C16 H36 N'
_chemical_formula_sum            'C16 H36 Cl3 N Sn'
_chemical_formula_weight         467.50
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-05-28 deposited with the CCDC.	2021-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.528(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7485(5)
_cell_length_b                   13.2735(5)
_cell_length_c                   18.4175(10)
_cell_measurement_reflns_used    7140
_cell_measurement_temperature    220.01(10)
_cell_measurement_theta_max      24.9880
_cell_measurement_theta_min      1.8800
_cell_volume                     2307.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      220.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.845
_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    -18.00  67.00   0.50   10.00    --  -11.40  45.00   1.96  170
  2  \w    -73.00  16.00   0.50   10.00    --  -11.40  45.00  93.02  178
  3  \w     31.00  78.00   0.50   10.00    --  -11.40  45.00  93.02   94
  4  \w    -98.00 -31.00   0.50   10.00    --  -11.40  45.00   1.96  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0324383000
_diffrn_orient_matrix_UB_12      0.0120197000
_diffrn_orient_matrix_UB_13      0.0293426000
_diffrn_orient_matrix_UB_21      -0.0312510000
_diffrn_orient_matrix_UB_22      -0.0486113000
_diffrn_orient_matrix_UB_23      -0.0030416000
_diffrn_orient_matrix_UB_31      0.0601353000
_diffrn_orient_matrix_UB_32      -0.0185968000
_diffrn_orient_matrix_UB_33      0.0267454000
_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  0.0174
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19216
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.998
_diffrn_reflns_theta_min         1.913
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.451
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.865
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         6208
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.001
_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^+3.3463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2097
_refine_ls_wR_factor_ref         0.2304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3848
_reflns_number_total             6208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02814f2.cif
_cod_data_source_block           mx9074
_cod_depositor_comments          'Adding full bibliography for 7128642.cif.'
_cod_database_code               7128642
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNClSn
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C5 = C6A-C5A = C7-C6A = C7-C6
 1.54 with sigma of 0.01
 C20-C19 = C20A-C19 = C21A-C20A = C21-C20
 1.54 with sigma of 0.02
 C19-C18
 1.54 with sigma of 0.01
 C21-C19
 2.5 with sigma of 0.02
 C19-C21A
 2.5 with sigma of 0.02
 C20A-C18
 2.5 with sigma of 0.02
 C18-C20
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C20 \\sim C21 \\sim C20A \\sim C21A: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.7A
C7 \\sim C6 \\sim C5 \\sim C6A \\sim C5A: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 1.7A
4. Others
 Sof(H7BC)=Sof(H7BD)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=
 Sof(H5AC)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(H5C)=FVAR(1)
 Sof(H19C)=Sof(H19D)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=1-FVAR(2)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H19A)=Sof(H19B)=Sof(C21)=Sof(H21A)=Sof(H21B)=
 Sof(H21C)=FVAR(2)
5.a Riding coordinates:
 C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C14(H14A,H14B), C8(H8A,H8B), C18(H18A,H18B),
 C15(H15A,H15B), C12(H12A,H12B), C16(H16A,H16B), C20(H20A,H20B), C7(H7AA,H7AB),
 C7(H7BC,H7BD), C19(H19A,H19B), C19(H19C,H19D), C6(H6A,H6B), C6A(H6AA,H6AB),
 C20A(H20C,H20D)
5.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC)
;
_shelx_res_checksum              38508
_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 1.464
_oxdiff_exptl_absorpt_empirical_full_min 0.622