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#$Date: 2023-05-05 05:15:28 +0300 (Fri, 05 May 2023) $
#$Revision: 283297 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/20/7712080.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7712080
loop_
_publ_author_name
'Bykowski, Janelle'
'Sinclair, Jocelyn'
'Trach, Jonathan'
'Ferguson, Michael J.'
'Rivard, Eric'
_publ_section_title
;
 Molecular Sn(II) precursors for room temperature deposition of
 crystalline elemental tin.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1602
_journal_page_last               1607
_journal_paper_doi               10.1039/d2dt04028j
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C16 H36 O4 Sn2'
_chemical_formula_sum            'C16 H36 O4 Sn2'
_chemical_formula_weight         529.83
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-12-13 deposited with the CCDC.	2023-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                114.7162(10)
_cell_angle_beta                 105.6759(11)
_cell_angle_gamma                96.9267(11)
_cell_formula_units_Z            1
_cell_length_a                   8.0779(7)
_cell_length_b                   8.3405(7)
_cell_length_c                   9.8156(8)
_cell_measurement_reflns_used    8345
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.44
_cell_volume                     557.38(8)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10236
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.558
_diffrn_reflns_theta_min         2.444
_diffrn_source                   'Short anode X-ray tube fine focus 2kW'
_exptl_absorpt_coefficient_mu    2.253
_exptl_absorpt_correction_T_max  0.7569
_exptl_absorpt_correction_T_min  0.5752
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       fragment
_exptl_crystal_F_000             264
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pentane'
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.208
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.059
_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     137
_refine_ls_number_reflns         3400
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0150
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0167P)²+0.1322P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0374
_refine_ls_wR_factor_ref         0.0380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3268
_reflns_number_total             3400
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt04028j2.cif
_cod_data_source_block           riv2272
_cod_depositor_comments
'Adding full bibliography for 7712080--7712083.cif.'
_cod_database_code               7712080
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.454
_shelx_estimated_absorpt_t_max   0.652
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.49928(2) -0.08389(2) 0.13381(2) 0.02687(3) Uani 1 1 d . . . . .
O1 O 0.58301(13) 0.15864(12) 0.11744(11) 0.02893(18) Uani 1 1 d . . . . .
O2 O 0.27211(14) -0.01896(16) 0.15109(14) 0.0366(2) Uani 1 1 d . . . . .
C1 C 0.6330(2) 0.34579(18) 0.24480(17) 0.0333(3) Uani 1 1 d . . . . .
C2 C 0.7802(3) 0.4574(2) 0.2257(2) 0.0533(5) Uani 1 1 d . . . . .
H2A H 0.817826 0.584024 0.311917 0.080 Uiso 1 1 calc R U . . .
H2B H 0.735373 0.455715 0.121659 0.080 Uiso 1 1 calc R U . . .
H2C H 0.882084 0.404330 0.231065 0.080 Uiso 1 1 calc R U . . .
C3 C 0.7025(3) 0.3448(3) 0.4048(2) 0.0517(4) Uani 1 1 d . . . . .
H3A H 0.740299 0.470578 0.492444 0.078 Uiso 1 1 calc R U . . .
H3B H 0.804354 0.291558 0.408940 0.078 Uiso 1 1 calc R U . . .
H3C H 0.607678 0.271547 0.415921 0.078 Uiso 1 1 calc R U . . .
C4 C 0.4697(3) 0.4202(2) 0.2321(3) 0.0517(4) Uani 1 1 d . . . . .
H4A H 0.501576 0.545816 0.319036 0.078 Uiso 1 1 calc R U . . .
H4B H 0.375526 0.343092 0.240636 0.078 Uiso 1 1 calc R U . . .
H4C H 0.426650 0.419680 0.128466 0.078 Uiso 1 1 calc R U . . .
C5 C 0.15572(19) -0.0740(2) 0.21876(17) 0.0354(3) Uani 1 1 d D . . . .
C6 C -0.0250(3) -0.1867(5) 0.0848(4) 0.0527(9) Uani 0.704(7) 1 d D U P A 1
H6A H -0.072952 -0.112424 0.036715 0.079 Uiso 0.704(7) 1 calc R U P A 1
H6B H -0.107940 -0.224061 0.129500 0.079 Uiso 0.704(7) 1 calc R U P A 1
H6C H -0.009955 -0.295776 0.002542 0.079 Uiso 0.704(7) 1 calc R U P A 1
C7 C 0.2208(4) -0.2014(7) 0.2855(6) 0.0728(15) Uani 0.704(7) 1 d D U P A 1
H7A H 0.228860 -0.311395 0.198915 0.109 Uiso 0.704(7) 1 calc R U P A 1
H7B H 0.136412 -0.236497 0.329917 0.109 Uiso 0.704(7) 1 calc R U P A 1
H7C H 0.338656 -0.137408 0.370105 0.109 Uiso 0.704(7) 1 calc R U P A 1
C8 C 0.1325(9) 0.0937(5) 0.3422(8) 0.108(3) Uani 0.704(7) 1 d D . P A 1
H8A H 0.247790 0.165761 0.428641 0.163 Uiso 0.704(7) 1 calc R U P A 1
H8B H 0.047927 0.058053 0.386227 0.163 Uiso 0.704(7) 1 calc R U P A 1
H8C H 0.086467 0.167471 0.292625 0.163 Uiso 0.704(7) 1 calc R U P A 1
C6A C 0.0390(17) -0.2616(10) 0.1027(12) 0.112(6) Uani 0.296(7) 1 d D U P A 2
H6D H 0.007184 -0.276831 -0.006509 0.168 Uiso 0.296(7) 1 calc R U P A 2
H6E H -0.069709 -0.279791 0.126798 0.168 Uiso 0.296(7) 1 calc R U P A 2
H6F H 0.102564 -0.351865 0.111241 0.168 Uiso 0.296(7) 1 calc R U P A 2
C7A C 0.2658(10) -0.041(2) 0.3848(9) 0.087(4) Uani 0.296(7) 1 d D U P A 2
H7D H 0.187923 -0.083309 0.430773 0.131 Uiso 0.296(7) 1 calc R U P A 2
H7E H 0.322996 0.090808 0.453766 0.131 Uiso 0.296(7) 1 calc R U P A 2
H7F H 0.357450 -0.107424 0.377097 0.131 Uiso 0.296(7) 1 calc R U P A 2
C8A C 0.0402(12) 0.0616(12) 0.2434(13) 0.061(2) Uani 0.296(7) 1 d D . P A 2
H8D H 0.117145 0.186806 0.312666 0.092 Uiso 0.296(7) 1 calc R U P A 2
H8E H -0.041175 0.034888 0.293858 0.092 Uiso 0.296(7) 1 calc R U P A 2
H8F H -0.029192 0.049726 0.139256 0.092 Uiso 0.296(7) 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Sn1 O1 89.83(4) . . ?
O2 Sn1 O1 92.93(4) . 2_655 ?
O1 Sn1 O1 72.78(4) . 2_655 ?
C1 O1 Sn1 126.37(8) . . ?
C1 O1 Sn1 123.82(8) . 2_655 ?
Sn1 O1 Sn1 107.22(4) . 2_655 ?
C5 O2 Sn1 129.22(9) . . ?
O1 C1 C2 108.05(12) . . ?
O1 C1 C4 108.88(12) . . ?
C2 C1 C4 111.21(15) . . ?
O1 C1 C3 108.20(12) . . ?
C2 C1 C3 109.81(15) . . ?
C4 C1 C3 110.59(15) . . ?
O2 C5 C6A 109.7(4) . . ?
O2 C5 C8 108.47(19) . . ?
O2 C5 C7A 108.6(3) . . ?
C6A C5 C7A 117.6(6) . . ?
O2 C5 C6 108.22(16) . . ?
C8 C5 C6 109.2(3) . . ?
O2 C5 C8A 104.8(3) . . ?
C6A C5 C8A 109.0(6) . . ?
C7A C5 C8A 106.4(5) . . ?
O2 C5 C7 112.28(15) . . ?
C8 C5 C7 112.8(3) . . ?
C6 C5 C7 105.7(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 O2 2.0051(10) . ?
Sn1 O1 2.1390(9) . ?
Sn1 O1 2.1544(9) 2_655 ?
O1 C1 1.4511(16) . ?
O2 C5 1.4226(16) . ?
C1 C2 1.522(2) . ?
C1 C4 1.522(2) . ?
C1 C3 1.522(2) . ?
C5 C6A 1.486(4) . ?
C5 C8 1.493(3) . ?
C5 C7A 1.517(4) . ?
C5 C6 1.530(3) . ?
C5 C8A 1.535(4) . ?
C5 C7 1.538(3) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sn1 O1 C1 C2 145.79(12) . . . . ?
Sn1 O1 C1 C2 -54.82(16) 2_655 . . . ?
Sn1 O1 C1 C4 -93.30(14) . . . . ?
Sn1 O1 C1 C4 66.09(14) 2_655 . . . ?
Sn1 O1 C1 C3 26.95(17) . . . . ?
Sn1 O1 C1 C3 -173.66(10) 2_655 . . . ?
Sn1 O2 C5 C6A -79.8(7) . . . . ?
Sn1 O2 C5 C8 125.1(4) . . . . ?
Sn1 O2 C5 C7A 50.0(6) . . . . ?
Sn1 O2 C5 C6 -116.5(2) . . . . ?
Sn1 O2 C5 C8A 163.3(5) . . . . ?
Sn1 O2 C5 C7 -0.2(3) . . . . ?
