Synthesis, characterisation and thermal properties of Sn(ii) pyrrolide complexes.
Parish, James D.; Snook, Michael W.; Johnson, Andrew L.; Kociok-Köhn, Gabriele; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7721–7729; doi:10.1039/c8dt00490k

data_7046171
_publ_section_title
;
 Synthesis, characterisation and thermal properties of Sn(ii) pyrrolide
 complexes.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7721
_journal_page_last               7729
_journal_paper_doi               10.1039/c8dt00490k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C13 H29 N3 Si2 Sn'
_chemical_formula_sum            'C13 H29 N3 Si2 Sn'
_chemical_formula_weight         402.26
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2018-01-30 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.431(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8512(4)
_cell_length_b                   10.4036(3)
_cell_length_c                   15.6557(5)
_cell_measurement_reflns_used    7054
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.8180
_cell_measurement_theta_min      3.8100
_cell_volume                     1918.13(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_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  84.00   1.00    2.50    --   16.99  57.00 -60.00   66
  2  \w      0.00  75.00   1.00    2.50    --   16.99  57.00 -90.00   75
  3  \w     -9.00  83.00   1.00    2.50    --   16.99  77.00  30.00   92
  4  \w    -30.00   8.00   1.00    2.50    --  -16.36  57.00 120.00   38
  5  \w    -52.00  35.00   1.00    2.50    --   16.99 -38.00 120.00   87
  6  \w    -58.00 -32.00   1.00    2.50    --  -16.36 113.00  91.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0479471000
_diffrn_orient_matrix_UB_12      -0.0071713000
_diffrn_orient_matrix_UB_13      0.0310645000
_diffrn_orient_matrix_UB_21      -0.0364246000
_diffrn_orient_matrix_UB_22      -0.0108630000
_diffrn_orient_matrix_UB_23      0.0322532000
_diffrn_orient_matrix_UB_31      0.0007701000
_diffrn_orient_matrix_UB_32      -0.0669349000
_diffrn_orient_matrix_UB_33      -0.0085821000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15655
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         3.270
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.451
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.403
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.293
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0167P)^2^+1.1343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3732
_reflns_number_total             4329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00490k2.cif
_cod_data_source_block           e15alj10
_cod_depositor_comments
'Adding full bibliography for 7046166--7046171.cif.'
_cod_database_code               7046171
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C13 H30 N3 Si2 Sn1'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C6(H6A,H6B,
 H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_olex2_date_sample_data_collection 2015-12-17
_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 1.087
_oxdiff_exptl_absorpt_empirical_full_min 0.925