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_4340588
_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 H21 Cl2 Ge P'
_chemical_formula_sum            'C21 H21 Cl2 Ge P'
_chemical_formula_weight         447.84
_chemical_name_common            4
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0720(3)
_cell_length_b                   9.3272(3)
_cell_length_c                   17.8199(5)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.29
_cell_volume                     2006.48(10)
_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'
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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  0.0159
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16975
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         2.286
_exptl_absorpt_coefficient_mu    1.874
_exptl_absorpt_correction_T_max  0.8375
_exptl_absorpt_correction_T_min  0.6602
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.156
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
; 
 Flack x determined using 2107 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.018(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4572
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0169
_refine_ls_R_factor_gt           0.0164
_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^)+(0.0247P)^2^+0.0757P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0435
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                4472
_reflns_number_total             4572
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           riv1355
_cod_depositor_comments
'Adding full bibliography for 4340585--4340595.cif.'
_cod_database_code               4340588
_shelx_estimated_absorpt_t_min   0.578
_shelx_estimated_absorpt_t_max   0.759
_shelxl_version_number           2013-2
_shelx_res_checksum              14767
_shelx_hkl_checksum              5753