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_7046167
_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         'C18 H26 N4 Sn'
_chemical_formula_sum            'C18 H26 N4 Sn'
_chemical_formula_weight         417.12
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-01-30 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.487(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1057(3)
_cell_length_b                   9.7711(2)
_cell_length_c                   16.0995(4)
_cell_measurement_reflns_used    6229
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.8460
_cell_measurement_theta_min      4.3950
_cell_volume                     1895.62(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_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 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12882
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.438
_diffrn_reflns_theta_min         4.375
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.746
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.728
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         3772
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0912P)^2^+1.0821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1453
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3460
_reflns_number_total             3772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00490k2.cif
_cod_data_source_block           s16alj19
_cod_depositor_comments
'Adding full bibliography for 7046166--7046171.cif.'
_cod_database_code               7046167
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.103
_shelx_estimated_absorpt_t_max   0.692
_oxdiff_exptl_absorpt_empirical_full_min 0.429
_oxdiff_exptl_absorpt_empirical_full_max 5.278
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4A-C26A \\sim N2-C6 \\sim N4-C26 \\sim N2A-C9A
 with sigma of 0.005
 Sn1-N4A \\sim Sn1-N2 \\sim Sn1-N4 \\sim Sn1-N2A
 with sigma of 0.005
 N3-C21 \\sim N3-C24A \\sim N3-C24 \\sim N3-C21A \\sim N1-C1 \\sim N1-C4A \\sim
N1-C1A \\sim N1-C4
 with sigma of 0.005
 C23A-C21A \\sim C24A-C22A
 with sigma of 0.005
 C2A-C1A \\sim C4-C3 \\sim C4A-C3A \\sim C2-C1 \\sim C22A-C21A \\sim C24-C23
\\sim C24A-C23A \\sim C22-C21
 with sigma of 0.005
 C3-C2 \\sim C3A-C2A
 with sigma of 0.005
 C4-C3 \\sim C2A-C1A \\sim C2-C1 \\sim C4A-C3A
 with sigma of 0.005
 C2A-C4A \\sim C1A-C3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) = Uanis(C1A)
Uanis(C4A) = Uanis(C1)
Uanis(C24A) = Uanis(C21)
Uanis(C21A) = Uanis(C24)
Uanis(C9A) = Uanis(C26)
Uanis(C26) = Uanis(C26A)
Uanis(C3A) = Uanis(C2)
Uanis(C2A) = Uanis(C3)
Uanis(C22A) = Uanis(C23)
Uanis(C22) = Uanis(C23A)
4. Others
 Fixed Sof: N4A(0.33) C21A(0.33) H21A(0.33) C22A(0.33) H22A(0.33) C23A(0.33)
 H23A(0.33) C24A(0.33) C25A(0.33) H25A(0.33) C26A(0.33) C27A(0.33) H27A(0.33)
 H27B(0.33) H27C(0.33) C28A(0.33) H28A(0.33) H28B(0.33) H28C(0.33) C29A(0.33)
 H29A(0.33) H29B(0.33) H29C(0.33) N4(0.67) N2(0.67) N2A(0.33) C24(0.67)
 C3A(0.33) H3A(0.33) C7A(0.33) H7AA(0.33) H7AB(0.33) H7AC(0.33) C28(0.67)
 H28D(0.67) H28E(0.67) H28F(0.67) C26(0.67) C1(0.67) H1(0.67) C1A(0.33)
 H1A(0.33) C2(0.67) H2(0.67) C5A(0.33) H5A(0.33) C3(0.67) H3(0.67) C9A(0.33)
 C4(0.67) C25(0.67) H25(0.67) C5(0.67) H5(0.67) C27(0.67) H27D(0.67) H27E(0.67)
 H27F(0.67) C6(0.67) C29(0.67) H29D(0.67) H29E(0.67) H29F(0.67) C7(0.67)
 H7A(0.67) H7B(0.67) H7C(0.67) C2A(0.33) H2A(0.33) C8(0.67) H8A(0.67) H8B(0.67)
 H8C(0.67) C4A(0.33) C9(0.67) H9A(0.67) H9B(0.67) H9C(0.67) C6A(0.33)
 H6AA(0.33) H6AB(0.33) H6AC(0.33) C21(0.67) H21(0.67) C8A(0.33) H8AA(0.33)
 H8AB(0.33) H8AC(0.33) C22(0.67) H22(0.67) C23(0.67) H23(0.67)
5.a Aromatic/amide H refined with riding coordinates:
 C21A(H21A), C22A(H22A), C23A(H23A), C25A(H25A), C3A(H3A), C1(H1), C1A(H1A),
 C2(H2), C5A(H5A), C3(H3), C25(H25), C5(H5), C2A(H2A), C21(H21), C22(H22),
 C23(H23)
5.b Idealised Me refined as rotating group:
 C27A(H27A,H27B,H27C), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C7A(H7AA,
 H7AB,H7AC), C28(H28D,H28E,H28F), C27(H27D,H27E,H27F), C29(H29D,H29E,H29F),
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C6A(H6AA,H6AB,H6AC),
 C8A(H8AA,H8AB,H8AC)
;
_shelx_res_checksum              9036