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_4340595
_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         'C21 H22 P, 0.5(C7 H8), Cl3 Sn'
_chemical_formula_sum            'C24.5 H26 Cl3 P Sn'
_chemical_formula_weight         576.46
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 97.060(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.368(9)
_cell_length_b                   13.284(6)
_cell_length_c                   18.748(9)
_cell_measurement_reflns_used    2294
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.97
_cell_measurement_theta_min      2.19
_cell_volume                     5034(4)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.1084
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17279
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.283
_diffrn_reflns_theta_min         1.834
_exptl_absorpt_coefficient_mu    1.407
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5643
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       needle
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.556
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.241
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0655
_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^)+(0.1020P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1582
_refine_ls_wR_factor_ref         0.1898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2628
_reflns_number_total             4559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501265k_si_002.cif
_cod_data_source_block           riv1393
_cod_depositor_comments
'Adding full bibliography for 4340585--4340595.cif.'
_cod_original_formula_sum        'C24.50 H26 Cl3 P Sn'
_cod_database_code               4340595
_shelx_estimated_absorpt_t_min   0.508
_shelx_estimated_absorpt_t_max   0.975
_shelxl_version_number           2013-2
_shelx_res_checksum              44099
_shelx_hkl_checksum              60292