Stabilization of the Heavy Methylene Analogues, GeH2 and SnH2, within the Coordination Sphere of a Transition Metal
S. M. Ibrahim Al-Rafia; Adam C. Malcolm; Sean K. Liew; Michael J. Ferguson; Eric Rivard; Journal of the American Chemical Society 133 (2011) 777–779; doi:10.1021/ja1106223

data_4105556
_publ_contact_author_address
;
Department of Chemistry
University of Alberta
Edmonton
AB T6G 2G2
CANADA
;
_publ_contact_author_email       ERIVARD@UALBERTA.CA
_publ_contact_author_name        'E. Rivard'
_publ_section_title
;
 Stabilization of the Heavy Methylene Analogues, GeH2 and SnH2, within the
 Coordination Sphere of a Transition Metal
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              777
_journal_page_last               779
_journal_paper_doi               10.1021/ja1106223
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C32 H38 N2 O5 Sn W, 0.25(C6 H14)'
_chemical_formula_sum            'C33.5 H41.5 N2 O5 Sn W'
_chemical_formula_weight         854.73
_chemical_name_common            'compound 3'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.330(6)
_cell_length_b                   19.457(8)
_cell_length_c                   26.718(10)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.23
_cell_volume                     7449(5)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            58643
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         27.69
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    3.793
_exptl_absorpt_correction_T_max  0.3604
_exptl_absorpt_correction_T_min  0.1683
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             3364
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.34
_refine_diff_density_max         3.143
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         8542
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0779P)^2^+28.8471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1600
_reflns_number_gt                7640
_reflns_number_total             8542
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja1106223_si_001_2.cif
_cod_data_source_block           riv1023
_cod_original_cell_volume        7450(5)
_cod_original_formula_sum        'C33.50 H41.50 N2 O5 Sn W'
_cod_database_code               4105556