Unsymmetrical Bicentric Organotin Lewis Acids {Me2N(CH2)3}Ph(X)Sn(CH2)nSnPh2X (X = F, I; n = 1, 3): Syntheses and Structures
Alashkar, Nour; Dietz, Christina; Baba Haj, Samer; Hiller, Wolf; Jurkschat, Klaus; Organometallics 35 (2016) 2738–; doi:10.1021/acs.organomet.6b00500

data_4088862
_publ_section_title
;
 Unsymmetrical Bicentric Organotin Lewis Acids
 {Me2N(CH2)3}Ph(X)Sn(CH2)nSnPh2X (X = F, I; n = 1, 3): Syntheses and
 Structures
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              2738
_journal_paper_doi               10.1021/acs.organomet.6b00500
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         '0.9(C30 H34 I N Sn2), 0.1(C24 H29 I2 N Sn2)'
_chemical_formula_sum            'C29.4 H33.5 I1.1 N Sn2'
_chemical_formula_weight         777.84
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.430(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3926(4)
_cell_length_b                   11.7904(4)
_cell_length_c                   23.7767(8)
_cell_measurement_reflns_used    9484
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.1619
_cell_measurement_theta_min      2.2901
_cell_volume                     2874.06(18)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.33.55'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.33.55'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.33.55'
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'enCIFer Version 1.5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XcaliburS CCD Diffractometer'
_diffrn_measurement_method       '\w und \y scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22890
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.415
_exptl_absorpt_coefficient_mu    2.937
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_description       prism
_exptl_crystal_F_000             1501
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.833
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5346
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0348P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3928
_reflns_number_total             5346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00500_si_002.cif
_cod_data_source_block           2046_compound-2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C29.40 H33.50 I1.10 N Sn2'
_cod_database_code               4088862
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              55097
_shelx_hkl_checksum              88208