Structural and electronic elucidation of N-heterocyclic silylene vanadocene adduct
Hänninen, Mikko; Baldansuren, Amgalanbaatar; Pugh, Thomas; Dalton Trans.  (2017) –; doi:10.1039/C7DT01226H

data_7042942
_publ_section_title
;
 Structural and electronic elucidation of N-heterocyclic silylene
 vanadocene adduct
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01226H
_journal_year                    2017
_chemical_formula_moiety         'C36 H46 N2 Si V'
_chemical_formula_sum            'C36 H46 N2 Si V'
_chemical_formula_weight         585.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-06-15 deposited with the CCDC.
2017-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                117.978(3)
_cell_angle_beta                 90.4725(19)
_cell_angle_gamma                91.1512(19)
_cell_formula_units_Z            4
_cell_length_a                   10.15070(15)
_cell_length_b                   18.9014(6)
_cell_length_c                   18.9172(6)
_cell_measurement_reflns_used    35390
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.9680
_cell_measurement_theta_min      3.7190
_cell_volume                     3204.02(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1636
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details
;
  1 omega  -25.00   50.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -        9.1007  -99.0000 -120.0000 75

  2 omega  -38.00   64.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       -9.5694   57.0000  120.0000 102

  3 omega  -83.00   19.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       -9.5694  -57.0000  -30.0000 102

  4 omega  -25.00   50.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -        9.1007  -99.0000   30.0000 75

  5 omega  -23.00   85.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -        9.1007   77.0000 -180.0000 108

  6 omega  -38.00   64.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       -9.5694   57.0000  -90.0000 102

  7 omega  -38.00   47.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       -9.5694   57.0000   60.0000 85

  8 omega  -25.00   31.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       -9.5694  -99.0000 -150.0000 56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0372704000
_diffrn_orient_matrix_UB_12      0.0016783000
_diffrn_orient_matrix_UB_13      0.0326575000
_diffrn_orient_matrix_UB_21      0.0574128000
_diffrn_orient_matrix_UB_22      -0.0098927000
_diffrn_orient_matrix_UB_23      -0.0235143000
_diffrn_orient_matrix_UB_31      0.0141930000
_diffrn_orient_matrix_UB_32      0.0413070000
_diffrn_orient_matrix_UB_33      0.0135584000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65256
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.083
_diffrn_reflns_theta_min         3.311
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  0.670
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.4766
_exptl_crystal_size_mid          0.4051
_exptl_crystal_size_min          0.378
_refine_diff_density_max         1.358
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         15096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0640P)^2^+6.2286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12304
_reflns_number_total             15096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01226h2.cif
_cod_data_source_block           oral304
_cod_database_code               7042942
_chemical_oxdiff_formula         'C36 H46 N2 Si1 V1'
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C21(H21), C24(H24), C9(H9), C61(H61), C49(H49), C64(H64), C52(H52)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C17(H17), C18(H18), C27(H27), C35(H35), C7(H7), C19(H19), C29(H29),
 C33(H33), C28(H28), C6(H6), C34(H34), C5(H5), C31(H31), C30(H30), C36(H36),
 C32(H32), C41(H41), C42(H42), C57(H57), C45(H45), C46(H46), C59(H59), C71(H71),
  C47(H47), C72(H72), C58(H58), C74(H74), C73(H73), C75(H75), C76(H76),
 C70(H70), C67(H67), C69(H69), C68(H68), C2(H2)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C10(H10A,H10B,H10C), C11(H11A,
 H11B,H11C), C51(H51A,H51B,H51C), C50(H50A,H50B,H50C), C66(H66A,H66B,H66C),
 C54(H54A,H54B,H54C), C63(H63A,H63B,H63C), C62(H62A,H62B,H62C), C53(H53A,H53B,
 H53C), C65(H65A,H65B,H65C)
;
_shelx_res_checksum              2078
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'