Germylene and Silylene Complexes of Molybdenum via E-H (E = Ge, Si) Bond Activations: Steric Influences on Intramolecular MoH...E Interactions
Akihiro Shinohara; Jennifer McBee; T. Don Tilley; Inorganic Chemistry 48 (2009) 8081–8083; doi:10.1021/ic901168s

data_4303107
_publ_section_title
;
Germylene and Silylene Complexes of Molybdenum via E-H (E = Ge, Si) Bond
Activations: Steric Influences on Intramolecular MoH...E Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8081
_journal_page_last               8083
_journal_paper_doi               10.1021/ic901168s
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C20 H42 Ge Mo P2'
_chemical_formula_sum            'C20 H42 Ge Mo P2'
_chemical_formula_weight         513.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.3120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7018(8)
_cell_length_b                   17.3143(15)
_cell_length_c                   16.3785(14)
_cell_measurement_reflns_used    6899
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      3.32
_cell_volume                     2410.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       q-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  0.0645
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11532
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs, 2004'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .07
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                3793
_reflns_number_total             4526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901168s_si_003.cif
_cod_data_source_block           aki9m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4303107