Triple bonds of niobium with silicon, germaniun and tin: the tetrylidyne complexes [(κ3-tmps)(CO)2NbE‒R] (E = Si, Ge, Sn; tmps = MeSi(CH2PMe2)3; R = aryl)
Filippou, Alexander C.; Hoffmann, David; Schnakenburg, Gregor; Chem. Sci.  (2017) –; doi:10.1039/C7SC02708G

data_1546541
_publ_section_title
;
 Triple bonds of niobium with silicon, germaniun and tin: the tetrylidyne
 complexes [(\k3-tmps)(CO)2Nb&#xE002;E--R] (E = Si, Ge, Sn; tmps =
 MeSi(CH2PMe2)3; R = aryl)
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC02708G
_journal_year                    2017
_chemical_formula_moiety         'C32 H30 Cl Ge Nb O3'
_chemical_formula_sum            'C32 H30 Cl Ge Nb O3'
_chemical_formula_weight         663.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-06-12 deposited with the CCDC.
2017-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.237(3)
_cell_length_b                   15.315(2)
_cell_length_c                   9.1804(13)
_cell_measurement_reflns_used    1732
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.41
_cell_volume                     2845.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_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  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11778
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    1.585
_exptl_absorpt_correction_T_max  0.9690
_exptl_absorpt_correction_T_min  0.8576
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker Sadabs 2009/2'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.1214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                2725
_reflns_number_total             3556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7sc02708g2.cif
_cod_data_source_block           3399f
_cod_original_cell_volume        2845.2(7)
_cod_database_code               1546541
_shelx_res_checksum              40971