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_1546543
_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_absolute_configuration ad
_chemical_formula_moiety         'C36 H52 Ge Nb O2 P3 Si, C4 H8 O'
_chemical_formula_sum            'C40 H60 Ge Nb O3 P3 Si'
_chemical_formula_weight         875.38
_chemical_name_systematic        DH-34-2
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-05-31 deposited with the CCDC.
2017-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.5480(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4180(3)
_cell_length_b                   22.9239(7)
_cell_length_c                   11.8653(5)
_cell_measurement_reflns_used    8273
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_cell_volume                     2183.14(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8273
_diffrn_reflns_point_group_measured_fraction_full 0.764
_diffrn_reflns_point_group_measured_fraction_max 0.764
_diffrn_reflns_theta_full        25.247
_diffrn_reflns_theta_max         25.247
_diffrn_reflns_theta_min         2.530
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.122
_exptl_absorpt_correction_T_max  0.8513
_exptl_absorpt_correction_T_min  0.7577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'R.H. Blessing, Acta Cryst. (1995), A51, 33-38'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Flack x determined using 1950 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6030
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.549
_reflns_Friedel_fraction_full    0.557
_reflns_Friedel_fraction_max     0.557
_reflns_number_gt                5739
_reflns_number_total             6030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc02708g2.cif
_cod_data_source_block           3550
_cod_database_code               1546543
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.662
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C28(H28A,H28B), C31(H31A,H31B), C37(H37A,H37B), C38(H38A,
 H38B), C39(H39A,H39B), C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C18(H18), C20(H20)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              97737
_olex2_submission_special_instructions 'No special instructions were received'