Synthesis and Characterization of N-[2-P(i-Pr)2-4-methylphenyl]2- (PNP) Pincer Tin(IV) and Tin(II) Complexes
Jens Henning; Hartmut Schubert; Klaus Eichele; Florian Winter; Rainer Pöttgen; Hermann August Mayer; Lars Wesemann; Inorganic Chemistry 51 (2012) 5787–5794; doi:10.1021/ic300324s

data_4329212
_publ_contact_author             'Lars Wesemann'
_publ_contact_author_address
;
Institut fuer Anorganische Chemie
Universitaet Tuebingen
Auf der Morgenstelle 18
72076 Tuebingen
Germany
;
_publ_contact_author_email       lars.wesemann@uni-tuebingen.de
_publ_contact_author_fax         0049-7071-292436
_publ_contact_author_phone       0049-7071-2976227
_publ_section_title
;
 Synthesis and Characterization of N-[2-P(i-Pr)2-4-methylphenyl]2- (PNP)
 Pincer Tin(IV) and Tin(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5787
_journal_page_last               5794
_journal_paper_doi               10.1021/ic300324s
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C32 H58 N2 P2 Si2 Sn'
_chemical_formula_sum            'C32 H58 N2 P2 Si2 Sn'
_chemical_formula_weight         707.61
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           shelxl-97
_cell_angle_alpha                84.389(2)
_cell_angle_beta                 85.663(2)
_cell_angle_gamma                71.484(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6494(3)
_cell_length_b                   10.6456(3)
_cell_length_c                   19.0757(5)
_cell_measurement_reflns_used    26170
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      59.25
_cell_measurement_theta_min      5.23
_cell_volume                     1847.12(9)
_computing_cell_refinement       x-Area
_computing_data_collection       x-Area
_computing_data_reduction        x-Area
_computing_molecular_graphics    'ortep for windows'
_computing_structure_refinement  'shelxl-97 (sheldrick, 1997)'
_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  'Stoe IPDS2'
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28135
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_T_max  0.9765
_exptl_absorpt_correction_T_min  0.8138
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'x-red, x-shape'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       needle
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         7839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(fo^2^)+(0.0339p)^2^+2.0763p] where p=(fo^2^+2fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                6848
_reflns_number_total             7839
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            ic300324s_si_001_1.cif
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_structure_factor_coef' value 'fsqd' changed to 'Fsqd'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_atom_site_adp_type'
value 'uani' changed to 'Uani' according to the built-in table from
CIF Core dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29 (40 times).

'_atom_site_adp_type' value 'uiso' changed to
'Uiso' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (65 times).

'_atom_site_refinement_flags' value 'r' changed to 'R'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (51 time).

'_atom_site_refinement_flags' value 'p' changed to 'P'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (2 times).

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_atom_site_refinement_flags' value 'pr' changed to 'PR' according to
the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (14 times).

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4329212