Vanadium(III) complexes incorporating the silylamino(disilylamido) ligand [(Me3Si)N{CH2CH2N(SiMe3)}2]2− [N{N″}2]2−. Synthesis and crystal structure of the dimeric, non-metallocene vanadium(III) hydride [{V(N{N″}2)}2(μ-H)2]
Clancy, Gerald P.; Clark, Howard C. S.; Clentsmith, Guy K. B.; Cloke, F. Geoffrey N.; Hitchcock, Peter B.; Journal of the Chemical Society, Dalton Transactions  (1999) 3345–; doi:10.1039/a904627e

data_7027596
_publ_section_title
;
 Vanadium(III) complexes incorporating the silylamino(disilylamido) ligand
 [(Me3Si)N{CH2CH2N(SiMe3)}2]2&#x2212; [N{N&#x2033;}2]2&#x2212;. Synthesis
 and crystal structure of the dimeric, non-metallocene vanadium(III)
 hydride [{V(N{N&#x2033;}2)}2(\m-H)2]
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_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3345
_journal_paper_doi               10.1039/a904627e
_journal_year                    1999
_chemical_formula_sum            'C26 H72 N6 Si6 V2'
_chemical_formula_weight         739.32
_chemical_name_common            '[V2(H)2{SiMe3N(CH2CH2NSiMe3)2}2]'
_chemical_name_systematic
; 
  ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 113.73
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.562(5)
_cell_length_b                   18.902(2)
_cell_length_c                   11.236
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     2053.5(10)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5193
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.998
_refine_ls_goodness_of_fit_obs   1.016
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_restrained_S_obs      1.016
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_obs          0.0480
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+1.5657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1265
_refine_ls_wR_factor_obs         0.1125
_reflns_number_observed          3800
_reflns_number_total             4946
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904627esup1.cif
_cod_data_source_block           feb1296
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+1.5657P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+1.5657P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027596