Application of the Donor-Acceptor Concept to Intercept Low Oxidation State Group 14 Element Hydrides using a Wittig Reagent as a Lewis Base.
Swarnakar, Anindya K.; McDonald, Sean M.; Deutsch, Kelsey C.; Choi, Paul; Ferguson, Michael J.; McDonald, Robert; Rivard, Eric; Inorganic chemistry 53 (2014) 8662–8671; doi:10.1021/ic501265k

data_4340594
_publ_section_title
;
 Application of the Donor-Acceptor Concept to Intercept Low Oxidation
 State Group 14 Element Hydrides using a Wittig Reagent as a Lewis Base.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8662
_journal_page_last               8671
_journal_paper_doi               10.1021/ic501265k
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C26 H23 O5 P Sn W, 0.5(C4 H10 O)'
_chemical_formula_sum            'C28 H28 O5.5 P Sn W'
_chemical_formula_weight         786.01
_chemical_name_common            10
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                79.1297(6)
_cell_angle_beta                 89.4825(7)
_cell_angle_gamma                64.8919(6)
_cell_formula_units_Z            2
_cell_length_a                   10.7586(6)
_cell_length_b                   11.9138(7)
_cell_length_c                   12.7748(8)
_cell_measurement_reflns_used    9071
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.53
_cell_measurement_theta_min      2.26
_cell_volume                     1451.45(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_unetI/netI     0.0106
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30449
_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         26.395
_diffrn_reflns_theta_min         1.628
_exptl_absorpt_coefficient_mu    4.911
_exptl_absorpt_correction_T_max  0.4311
_exptl_absorpt_correction_T_min  0.2513
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_description       block
_exptl_crystal_F_000             758
_exptl_crystal_size_max          0.452
_exptl_crystal_size_mid          0.328
_exptl_crystal_size_min          0.282
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5932
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0169
_refine_ls_R_factor_gt           0.0167
_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^)+(0.0208P)^2^+1.4870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5850
_reflns_number_total             5932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501265k_si_002.cif
_cod_data_source_block           riv1435
_cod_depositor_comments
'Adding full bibliography for 4340585--4340595.cif.'
_cod_original_formula_sum        'C28 H28 O5.50 P Sn W'
_cod_database_code               4340594
_shelx_estimated_absorpt_t_min   0.215
_shelx_estimated_absorpt_t_max   0.338
_shelxl_version_number           2013-4
_shelx_res_checksum              97931
_shelx_hkl_checksum              64782