Amine-directed synthesis, valence state control, and optical properties of two new organic-inorganic tin chlorides.
Wen, Xuemei; Yi, Gangji; Zhang, Zhizhuan; Guo, Caihong; Zeng, Hongmei; Huang, Ling; Zou, Guohong; Lin, Zhien; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13195–13200; doi:10.1039/d4dt01919a

data_7716701
_publ_section_title
;
 Amine-directed synthesis, valence state control, and optical properties
 of two new organic-inorganic tin chlorides.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13195
_journal_page_last               13200
_journal_paper_doi               10.1039/d4dt01919a
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         '2(Cl2 Sn0.5), Cl, C9 H26 N3'
_chemical_formula_sum            'C9 H26 Cl5 N3 Sn'
_chemical_formula_weight         472.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-07-03 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6468(5)
_cell_length_b                   11.6876(3)
_cell_length_c                   11.4470(3)
_cell_measurement_reflns_used    1782
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5980
_cell_measurement_theta_min      3.9070
_cell_volume                     1825.78(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -86.00 -41.00   1.00    3.00    --  -15.32-178.00   0.00   45
  2  \w     -4.00  26.00   1.00    3.00    --   17.59  77.00 -90.00   30
  3  \w     12.00  75.00   1.00    3.00    --   17.59  38.00-150.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0433370000
_diffrn_orient_matrix_UB_12      0.0054449000
_diffrn_orient_matrix_UB_13      0.0337895000
_diffrn_orient_matrix_UB_21      0.0260697000
_diffrn_orient_matrix_UB_22      0.0323580000
_diffrn_orient_matrix_UB_23      0.0421601000
_diffrn_orient_matrix_UB_31      -0.0119255000
_diffrn_orient_matrix_UB_32      0.0510804000
_diffrn_orient_matrix_UB_33      -0.0303241000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2529
_diffrn_reflns_point_group_measured_fraction_full 0.715
_diffrn_reflns_point_group_measured_fraction_max 0.701
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.904
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.120
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.718
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 311 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_coef       0.0026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1368
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+0.4075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.332
_reflns_Friedel_fraction_full    0.398
_reflns_Friedel_fraction_max     0.369
_reflns_number_gt                1332
_reflns_number_total             1368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01919a2.cif
_cod_data_source_block           xm3-24-5_auto
_cod_depositor_comments
'Adding full bibliography for 7716701--7716702.cif.'
_cod_database_code               7716701
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.609
_shelx_estimated_absorpt_t_min   0.516
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5)
 H4B(0.5) C3'(0.5) H3'A(0.5) H3'B(0.5) C4'(0.5) H4'A(0.5) H4'B(0.5) H5A(0.5)
 H5B(0.5) H5C(0.5)
3.a Riding coordinates:
 C5(H5A,H5B,H5C)
3.b Ternary CH refined with riding coordinates:
 N1(H1A), N1(H1B), N2(H2)
3.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C3'(H3'A,H3'B), C4'(H4'A,H4'B)
3.d Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              73774
_shelx_hkl_checksum              76897
_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 1.119
_oxdiff_exptl_absorpt_empirical_full_min 0.895