Tin Guanidinato Complexes: Oxidative Control of Sn, SnS, SnSe and SnTe Thin Film Deposition
Johnson, Andrew Lee; Ahmet, Ibrahim Y.; Hill, Michael S.; Raithby, Paul R.; Dalton Transactions  (2018) –; doi:10.1039/C8DT00773J

data_7045814
_publ_section_title
;
 Tin Guanidinato Complexes: Oxidative Control of Sn, SnS, SnSe and SnTe
 Thin Film Deposition
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT00773J
_journal_year                    2018
_chemical_formula_moiety         'C30 H56 N6 S4 Sn, 0.17(C6 H14)'
_chemical_formula_sum            'C31 H58.33 N6 S4 Sn'
_chemical_formula_weight         762.10
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-03 deposited with the CCDC.
2018-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.4110(7)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   34.0180(6)
_cell_length_b                   10.6170(2)
_cell_length_c                   43.7820(8)
_cell_measurement_reflns_used    113335
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      0.970
_cell_volume                     15168.5(5)
_computing_cell_refinement       KappaCCD
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Kappa Nonius'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0988
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            109659
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         1.248
_diffrn_source                   'Sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SOTRAV, Blessing (1985)'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             6405
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.917
_exptl_transmission_factor_min   0.689
_refine_diff_density_max         1.296
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       0.00121(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         17377
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0449
_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^)+(0.1209P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13069
_reflns_number_total             17416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00773j2.cif
_cod_data_source_block           11
_cod_database_code               7045814
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.837
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C121-C122 \\sim C122-C123 \\sim C123-C124 \\sim C124-C125 \\sim C125-C126
\\sim C126-C121
 with sigma of 0.02
 C127-C128 \\sim C128-C129 \\sim C129-C130 \\sim C130-C131 \\sim C131-C132
\\sim C132-C127
 with sigma of 0.02
 C221-C222 \\sim C222-C223 \\sim C223-C224 \\sim C224-C225 \\sim C225-C226
\\sim C226-C221
 with sigma of 0.02
 C227-C228 \\sim C228-C229 \\sim C229-C230 \\sim C230-C231 \\sim C231-C232
\\sim C232-C227
 with sigma of 0.02
3. Same fragment restrains
{C421, C422, C423, C424, C425, C426} sigma for 1-2: 0.02, 1-3: 0.04
as
{C221, C222, C223, C224, C225, C226}
{C421, C422, C423, C424, C425, C426} sigma for 1-2: 0.02, 1-3: 0.04
as
{C227, C228, C229, C230, C231, C232}
4. Others
 Sof(C127)=Sof(H127)=Sof(C128)=Sof(H12K)=Sof(H12L)=Sof(C129)=Sof(H12M)=
 Sof(H12N)=Sof(C130)=Sof(H13A)=Sof(H13B)=Sof(C131)=Sof(H13C)=Sof(H13D)=
 Sof(C132)=Sof(H13E)=Sof(H13F)=1-FVAR(1)
 Sof(C121)=Sof(H121)=Sof(C122)=Sof(H12A)=Sof(H12B)=Sof(C123)=Sof(H12C)=
 Sof(H12D)=Sof(C124)=Sof(H12E)=Sof(H12F)=Sof(C125)=Sof(H12G)=Sof(H12H)=
 Sof(C126)=Sof(H12I)=Sof(H12J)=FVAR(1)
 Sof(C227)=Sof(H227)=Sof(C228)=Sof(H22K)=Sof(H22L)=Sof(C229)=Sof(H22M)=
 Sof(H22N)=Sof(C230)=Sof(H23A)=Sof(H23B)=Sof(C231)=Sof(H23C)=Sof(H23D)=
 Sof(C232)=Sof(H23E)=Sof(H23F)=1-FVAR(2)
 Sof(C221)=Sof(H221)=Sof(C222)=Sof(H22A)=Sof(H22B)=Sof(C223)=Sof(H22C)=
 Sof(H22D)=Sof(C224)=Sof(H22E)=Sof(H22F)=Sof(C225)=Sof(H22G)=Sof(H22H)=
 Sof(C226)=Sof(H22I)=Sof(H22J)=FVAR(2)
 Fixed Sof: C61(0.33333) H61A(0.33333) H61B(0.33333) H61C(0.33333)
 C62(0.33333) H62A(0.33333) H62B(0.33333) C63(0.33333) H63A(0.33333)
 H63B(0.33333) C64(0.33333) H64A(0.33333) H64B(0.33333) C65(0.33333)
 H65A(0.33333) H65B(0.33333) C66(0.33333) H66A(0.33333) H66B(0.33333)
 H66C(0.33333)
5.a Ternary CH refined with riding coordinates:
 C111(H111), C121(H121), C127(H127), C211(H211), C221(H221), C227(H227),
 C311(H311), C321(H321), C411(H411), C421(H421)
5.b Secondary CH2 refined with riding coordinates:
 C112(H11A,H11B), C113(H11C,H11D), C114(H11E,H11F), C115(H11G,H11H), C116(H11I,
 H11J), C122(H12A,H12B), C123(H12C,H12D), C124(H12E,H12F), C125(H12G,H12H),
 C126(H12I,H12J), C128(H12K,H12L), C129(H12M,H12N), C130(H13A,H13B), C131(H13C,
 H13D), C132(H13E,H13F), C212(H21A,H21B), C213(H21C,H21D), C214(H21E,H21F),
 C215(H21G,H21H), C216(H21I,H21J), C222(H22A,H22B), C223(H22C,H22D), C224(H22E,
 H22F), C225(H22G,H22H), C226(H22I,H22J), C228(H22K,H22L), C229(H22M,H22N),
 C230(H23A,H23B), C231(H23C,H23D), C232(H23E,H23F), C312(H31A,H31B), C313(H31C,
 H31D), C314(H31E,H31F), C315(H31G,H31H), C316(H31I,H31J), C322(H32A,H32B),
 C323(H32C,H32D), C324(H32E,H32F), C325(H32G,H32H), C326(H32I,H32J), C412(H41A,
 H41B), C413(H41C,H41D), C414(H41E,H41F), C415(H41G,H41H), C416(H41I,H41J),
 C422(H42A,H42B), C423(H42C,H42D), C424(H42E,H42F), C425(H42G,H42H), C426(H42I,
 H42J), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C61(H61A,H61B,
 H61C), C66(H66A,H66B,H66C)
;
_olex2_submission_special_instructions 'No special instructions were received'