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_7045813
_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 Se Sn'
_chemical_formula_sum            'C30 H56 N6 Se Sn'
_chemical_formula_weight         698.45
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 103.1790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2422(3)
_cell_length_b                   26.8816(3)
_cell_length_c                   12.4038(6)
_cell_measurement_reflns_used    43124
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      27.734
_cell_measurement_theta_min      1.515
_cell_volume                     3974.5(2)
_computing_cell_refinement       'Nonius Kappa'
_computing_data_collection       'Nonius Kappa'
_computing_data_reduction        'Nonius Kappa'
_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 0.974
_diffrn_measured_fraction_theta_max 0.957
_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  0.1157
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            43124
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.734
_diffrn_reflns_theta_min         1.515
_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    1.582
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Semi-empirical
_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    1.167
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.857
_refine_diff_density_max         0.626
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         8952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0769P)^2^+7.2822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7653
_reflns_number_total             8952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00773j2.cif
_cod_data_source_block           16
_cod_database_code               7045813
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.797
_shelx_estimated_absorpt_t_min   0.743
_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.a Ternary CH refined with riding coordinates:
 C111(H111), C121(H121), C211(H211), C221(H221)
2.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), 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)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_olex2_submission_original_sample_id h13alj16
_olex2_submission_special_instructions 'No special instructions were received'