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_1546542
_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         'C36 H52 Nb O2 P3 Si Sn, C7 H8'
_chemical_formula_sum            'C43 H60 Nb O2 P3 Si Sn'
_chemical_formula_weight         941.51
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     heavy
_audit_creation_date             2014-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2017-05-31 deposited with the CCDC.
2017-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.779(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5148(6)
_cell_length_b                   23.2579(16)
_cell_length_c                   12.0766(8)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.87
_cell_measurement_theta_min      2.50
_cell_volume                     2264.3(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_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  0.0408
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20515
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.725
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5373
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0889 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.7202.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.403
_refine_diff_density_min         -2.852
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         10697
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0703
_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^)+(0.0103P)^2^+27.6525P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                9665
_reflns_number_total             10697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc02708g2.cif
_cod_data_source_block           3697f
_cod_database_code               1546542
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.893
_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. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C12)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C28(H28A,H28B), C31(H31A,H31B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C18(H18), C20(H20), C38(H38),
 C39(H39), C40(H40), C41(H41), C42(H42)
3.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), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              18154
_olex2_submission_special_instructions 'No special instructions were received'