Synthesis and structures of halides and pseudohalides of bis[2,6-bis(dimethylamino)phenyl]tin(IV)
Hitchcock, Peter B.; Lappert, Michael F.; Protchenko, Andrey V.; Uiterweerd, Patrick G. H.; Dalton Transactions  (2009) 353–361; doi:10.1039/b813353k

data_7030546
_publ_section_title
;
 Synthesis and structures of halides and pseudohalides of
 bis[2,6-bis(dimethylamino)phenyl]tin(IV)
;
_journal_coden_ASTM              DTARAF
_journal_issue                   2
_journal_name_full               'Dalton Transactions'
_journal_page_first              353
_journal_page_last               361
_journal_paper_doi               10.1039/b813353k
_journal_year                    2009
_chemical_formula_moiety         'C10 H15 Cl N2 Sn'
_chemical_formula_sum            'C10 H15 Cl N2 Sn'
_chemical_formula_weight         317.38
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.12(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.135(1)
_cell_length_b                   9.190(1)
_cell_length_c                   15.934(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      8.5
_cell_measurement_theta_min      7.3
_cell_measurement_wavelength     0.71073
_cell_volume                     1191.0(3)
_computing_cell_refinement       'CAD4 (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5499
_diffrn_reflns_theta_full        34.97
_diffrn_reflns_theta_max         34.97
_diffrn_reflns_theta_min         2.50
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        7
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.335
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was 1
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.227
_refine_diff_density_min         -1.893
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       0.0041(6)
_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_all   1.150
_refine_ls_goodness_of_fit_obs   1.218
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         5220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_restrained_S_obs      1.218
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_obs          0.0598
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+4.7162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1442
_refine_ls_wR_factor_obs         0.1352
_reflns_number_observed          4105
_reflns_number_total             5220
_reflns_observed_criterion       >2sigma(I)
_cod_duplicate_entry             7000260
_cod_data_source_file            b813353k.txt
_cod_data_source_block           (2)-may798
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7030546
_diffrn_standards_decay_corr_max 1.073
_diffrn_standards_decay_corr_min 0.996