Isomeric Forms of Divalent Heavier Group 14 Element Hydrides: Characterization of Ar'(H)GeGe(H)Ar' and Ar'(H)2GeGeAr'.PMe3 (Ar' = C6H3-2,6-Dipp2; Dipp = C6H3-2,6-Pri2)
Anne F. Richards; Andrew D. Phillips; Marilyn M. Olmstead; Philip P. Power; Journal of the American Chemical Society 125 (2003) 3204–3205; doi:10.1021/ja029772g

data_4113570
_publ_section_title
;
 Isomeric Forms of Divalent Heavier Group 14 Element Hydrides:
 Characterization of Ar'(H)GeGe(H)Ar' and Ar'(H)2GeGeAr'.PMe3 (Ar' =
 C6H3-2,6-Dipp2; Dipp = C6H3-2,6-Pri2)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3204
_journal_page_last               3205
_journal_paper_doi               10.1021/ja029772g
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         C63H82Ge2P,0.5C6H14
_chemical_formula_sum            'C66 H89 Ge2 P'
_chemical_formula_weight         1058.52
_chemical_melting_point          364
_chemical_name_common            DippH2GeGeDippPMe3.0.5n-hexane
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 107.251(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.114(4)
_cell_length_b                   37.253(11)
_cell_length_c                   12.614(4)
_cell_measurement_reflns_used    699
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.7
_cell_volume                     5885(3)
_computing_cell_refinement       'SMART 5.054 (Bruker, 2001)'
_computing_data_collection       'SMART 5.054 (Bruker, 2001)'
_computing_data_reduction        'SAINT 6.33 (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            76914
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        <0.1
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    1.086
_exptl_absorpt_correction_T_max  0.7654
_exptl_absorpt_correction_T_min  0.6704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.04 (Sheldrick, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.424
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         17830
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+14.5029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1434
_reflns_number_gt                14724
_reflns_number_total             17830
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja029772gsi20030124_045200.cif
_cod_data_source_block           ar02
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4113570