Formation and Structure of fac-[Mo(CO)3(C2H2[N(CH2But)]2Ge)3]: The First Structurally Characterized Group 6 Transition Metal Complex of an Unsaturated Diaminogermylene
Olaf Kühl; Peter Lönnecke; Joachim Heinicke; Inorganic Chemistry 42 (2003) 2836–2838; doi:10.1021/ic0259991

data_4313550
_publ_section_title
;
 Formation and Structure of fac-[Mo(CO)3(C2H2[N(CH2But)]2Ge)3]: The First
 Structurally Characterized Group 6 Transition Metal Complex of an
 Unsaturated Diaminogermylene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2836
_journal_page_last               2838
_journal_paper_doi               10.1021/ic0259991
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C39 H72 Ge3 Mo N6 O3'
_chemical_formula_weight         986.74
_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                 96.398(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.525(3)
_cell_length_b                   10.5325(17)
_cell_length_c                   23.949(4)
_cell_measurement_reflns_used    1200
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      1.05
_cell_volume                     4894.4(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega 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  0.0894
_diffrn_reflns_av_sigmaI/netI    0.1115
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28765
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    2.112
_exptl_absorpt_correction_T_max  0.8165
_exptl_absorpt_correction_T_min  0.6773
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.031
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         10011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.1387
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0702P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1460
_reflns_number_gt                5201
_reflns_number_total             10011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0259991si20020904_051616.cif
_cod_data_source_block           c982_fin
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4894.4(13)
_cod_database_code               4313550