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_4105555
_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         'C53 H56 N2 O8 Sn W, C4 H10 O'
_chemical_formula_sum            'C57 H66 N2 O9 Sn W'
_chemical_formula_weight         1225.66
_chemical_name_common            'compound 6'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   17.910(4)
_cell_length_b                   13.236(3)
_cell_length_c                   23.515(5)
_cell_measurement_reflns_used    9423
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.43
_cell_volume                     5574(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            47549
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    2.564
_exptl_absorpt_correction_T_max  0.7186
_exptl_absorpt_correction_T_min  0.4554
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881. 6222 Friedel pairs'
_refine_ls_abs_structure_Flack   0.006(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         12822
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0000P)^2^+3.2027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0515
_reflns_number_gt                12002
_reflns_number_total             12822
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja1106223_si_001_1.cif
_cod_data_source_block           riv1077
_cod_original_cell_volume        5575(2)
_cod_database_code               4105555