#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/12/4321233.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4321233
loop_
_publ_author_name
'Sian C. Davies'
'David L. Hughes'
'Zofia Janas'
'Lucjan B. Jerzykiewicz'
'Raymond L. Richards'
'J. Roger Sanders'
'James E. Silverston'
'Piotr Sobota'
_publ_section_title
;
 Vanadium Complexes of the N(CH2CH2S)33- and O(CH2CH2S)22- Ligands with
 Coligands Relevant to Nitrogen Fixation Processes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3485
_journal_page_last               3498
_journal_paper_doi               10.1021/ic9909476
_journal_volume                  39
_journal_year                    2000
_chemical_formula_structural     '[V {O(CH2CH2S)2} (NSiMe3) (dipp)]'
_chemical_formula_sum            'C19 H34 N O2 S2 Si V'
_chemical_formula_weight         451.62
_chemical_name_common            'Compound 16'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.06(3)
_cell_angle_beta                 102.12(3)
_cell_angle_gamma                118.16(3)
_cell_formula_units_Z            2
_cell_length_a                   9.646(2)
_cell_length_b                   10.103(2)
_cell_length_c                   15.001(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     1248.4(6)
_computing_cell_refinement       'Kuma KM4 software 1996'
_computing_data_collection       'Kuma KM4 software 1996'
_computing_data_reduction        'Kuma KM4 software 1996'
_computing_molecular_graphics    'ORTEPII, 1976'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      302(2)
_diffrn_measured_fraction_theta_full 0.576
_diffrn_measured_fraction_theta_max 0.576
_diffrn_measurement_device       'Kuma KM4 automatic diffractometer'
_diffrn_measurement_method       'profile data from omega/2theta scans'
_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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2746
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        21.3
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       orange
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_obs          0.0516
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1153P)²+1.1750P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1719
_refine_ls_wR_factor_obs         0.1653
_reflns_number_gt                2236
_reflns_number_total             2541
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9909476_13.cif
_cod_data_source_block           C19H34NO2SiS2V
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1153P)^2^+1.1750P] 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^)+(0.1153P)^2^+1.1750P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1248.4(4)
_cod_original_formula_sum        'C19 H34 N O2 Si S2 V'
_cod_database_code               4321233
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V V 0.38467(11) 0.63138(10) 0.64515(6) 0.0477(4) Uani 1 d . . .
S1 S 0.3591(2) 0.39873(19) 0.62261(12) 0.0635(5) Uani 1 d . . .
S2 S 0.5260(2) 0.8121(2) 0.56381(13) 0.0670(5) Uani 1 d . . .
SI Si 0.7053(2) 0.7383(2) 0.82761(14) 0.0859(6) Uani 1 d . . .
O1 O 0.2020(5) 0.5440(5) 0.5115(3) 0.0671(11) Uani 1 d . . .
O2 O 0.2295(4) 0.6489(4) 0.6856(2) 0.0496(9) Uani 1 d . . .
N N 0.5358(6) 0.6875(5) 0.7364(3) 0.0591(12) Uani 1 d . . .
C1 C 0.1946(10) 0.4200(9) 0.4582(5) 0.090(2) Uani 1 d . . .
C2 C 0.1932(10) 0.3088(8) 0.5203(5) 0.087(2) Uani 1 d . . .
C3 C 0.2125(12) 0.6660(11) 0.4608(6) 0.101(3) Uani 1 d . . .
C4 C 0.3790(11) 0.7625(10) 0.4525(5) 0.093(2) Uani 1 d . . .
C5 C 0.7197(14) 0.5694(12) 0.8484(8) 0.145(4) Uani 1 d . . .
C6 C 0.6755(18) 0.8228(18) 0.9254(7) 0.208(8) Uani 1 d . . .
C7 C 0.8809(15) 0.8795(18) 0.7902(12) 0.231(9) Uani 1 d . . .
C11 C 0.2299(7) 0.6939(6) 0.7726(3) 0.0491(13) Uani 1 d . . .
C12 C 0.1670(7) 0.5823(7) 0.8295(4) 0.0585(15) Uani 1 d . . .
C13 C 0.1685(9) 0.6331(9) 0.9163(4) 0.0725(18) Uani 1 d . . .
C14 C 0.2285(10) 0.7818(10) 0.9458(5) 0.083(2) Uani 1 d . . .
C15 C 0.2899(9) 0.8884(9) 0.8897(5) 0.0753(18) Uani 1 d . . .
C16 C 0.2922(7) 0.8487(6) 0.8009(4) 0.0551(14) Uani 1 d . . .
C120 C 0.1002(9) 0.4169(7) 0.7967(5) 0.0736(18) Uani 1 d . . .
C121 C -0.0768(10) 0.3216(9) 0.7986(6) 0.101(3) Uani 1 d . . .
C122 C 0.2068(12) 0.3566(10) 0.8495(7) 0.115(3) Uani 1 d . . .
C160 C 0.3584(8) 0.9651(7) 0.7382(4) 0.0630(16) Uani 1 d . . .
C161 C 0.2264(10) 0.9659(9) 0.6667(6) 0.103(3) Uani 1 d . . .
C162 C 0.4750(11) 1.1245(9) 0.7891(6) 0.105(3) Uani 1 d . . .
H1A H 0.2880 0.4558 0.4322 0.108 Uiso 1 calc R . .
H1B H 0.0971 0.3742 0.4082 0.108 Uiso 1 calc R . .
H2A H 0.2028 0.2302 0.4884 0.104 Uiso 1 calc R . .
H2B H 0.0909 0.2616 0.5378 0.104 Uiso 1 calc R . .
H3A H 0.1784 0.7264 0.4918 0.121 Uiso 1 calc R . .
H3B H 0.1398 0.6249 0.3999 0.121 Uiso 1 calc R . .
H4A H 0.3879 0.8544 0.4292 0.111 Uiso 1 calc R . .
H4B H 0.4034 0.7096 0.4089 0.111 Uiso 1 calc R . .
H5A H 0.8136 0.5945 0.8973 0.174 Uiso 1 calc R . .
H5B H 0.7290 0.5273 0.7935 0.174 Uiso 1 calc R . .
H5C H 0.6241 0.4966 0.8653 0.174 Uiso 1 calc R . .
H6A H 0.7637 0.8473 0.9781 0.250 Uiso 1 calc R . .
H6B H 0.5751 0.7522 0.9387 0.250 Uiso 1 calc R . .
H6C H 0.6721 0.9135 0.9107 0.250 Uiso 1 calc R . .
H7A H 0.9058 0.8303 0.7456 0.277 Uiso 1 calc R . .
H7B H 0.9726 0.9287 0.8423 0.277 Uiso 1 calc R . .
H7C H 0.8559 0.9535 0.7631 0.277 Uiso 1 calc R . .
H13 H 0.1269 0.5625 0.9558 0.087 Uiso 1 calc R . .
H14 H 0.2277 0.8113 1.0047 0.100 Uiso 1 calc R . .
H15 H 0.3311 0.9900 0.9113 0.090 Uiso 1 calc R . .
H120 H 0.1047 0.4094 0.7322 0.088 Uiso 1 calc R . .
H12A H -0.0850 0.3173 0.8612 0.121 Uiso 1 calc R . .
H12B H -0.1189 0.2209 0.7683 0.121 Uiso 1 calc R . .
H12C H -0.1384 0.3664 0.7673 0.121 Uiso 1 calc R . .
H12D H 0.1807 0.2617 0.8171 0.139 Uiso 1 calc R . .
H12E H 0.1881 0.3419 0.9098 0.139 Uiso 1 calc R . .
H12F H 0.3189 0.4282 0.8548 0.139 Uiso 1 calc R . .
H160 H 0.4202 0.9356 0.7061 0.076 Uiso 1 calc R . .
H16A H 0.2728 1.0373 0.6259 0.123 Uiso 1 calc R . .
H16B H 0.1628 0.9943 0.6957 0.123 Uiso 1 calc R . .
H16C H 0.1583 0.8666 0.6323 0.123 Uiso 1 calc R . .
H16D H 0.5635 1.1239 0.8322 0.127 Uiso 1 calc R . .
H16E H 0.4185 1.1577 0.8215 0.127 Uiso 1 calc R . .
H16F H 0.5161 1.1924 0.7456 0.127 Uiso 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N V O2 104.48(19) . . ?
N V O1 171.11(19) . . ?
O2 V O1 84.28(16) . . ?
N V S1 93.63(17) . . ?
O2 V S1 118.39(14) . . ?
O1 V S1 80.66(13) . . ?
N V S2 94.97(19) . . ?
O2 V S2 117.00(13) . . ?
O1 V S2 82.08(14) . . ?
S1 V S2 119.34(8) . . ?
C2 S1 V 102.8(3) . . ?
C4 S2 V 102.5(3) . . ?
N SI C5 107.6(4) . . ?
N SI C6 107.0(4) . . ?
C5 SI C6 113.5(7) . . ?
N SI C7 106.2(5) . . ?
C5 SI C7 111.7(8) . . ?
C6 SI C7 110.4(9) . . ?
C3 O1 C1 113.9(6) . . ?
C3 O1 V 110.7(5) . . ?
C1 O1 V 115.7(4) . . ?
C11 O2 V 129.8(3) . . ?
V N SI 174.1(3) . . ?
O1 C1 C2 107.5(6) . . ?
C1 C2 S1 110.9(5) . . ?
O1 C3 C4 111.0(6) . . ?
C3 C4 S2 111.2(5) . . ?
O2 C11 C16 118.8(5) . . ?
O2 C11 C12 118.4(5) . . ?
C16 C11 C12 122.8(5) . . ?
C13 C12 C11 116.2(6) . . ?
C13 C12 C120 122.4(6) . . ?
C11 C12 C120 121.4(5) . . ?
C14 C13 C12 122.4(6) . . ?
C13 C14 C15 120.5(6) . . ?
C14 C15 C16 121.5(7) . . ?
C15 C16 C11 116.6(6) . . ?
C15 C16 C160 122.0(6) . . ?
C11 C16 C160 121.4(5) . . ?
C12 C120 C121 112.4(6) . . ?
C12 C120 C122 111.0(7) . . ?
C121 C120 C122 112.3(6) . . ?
C161 C160 C16 111.7(6) . . ?
C161 C160 C162 110.2(6) . . ?
C16 C160 C162 113.6(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V N 1.635(5) . ?
V O2 1.808(3) . ?
V O1 2.210(4) . ?
V S1 2.256(2) . ?
V S2 2.261(2) . ?
S1 C2 1.813(8) . ?
S2 C4 1.831(8) . ?
SI N 1.747(5) . ?
SI C5 1.803(9) . ?
SI C6 1.823(10) . ?
SI C7 1.835(12) . ?
O1 C3 1.435(9) . ?
O1 C1 1.438(8) . ?
O2 C11 1.373(6) . ?
C1 C2 1.470(11) . ?
C3 C4 1.468(12) . ?
C11 C16 1.403(8) . ?
C11 C12 1.406(8) . ?
C12 C13 1.385(9) . ?
C12 C120 1.507(9) . ?
C13 C14 1.355(10) . ?
C14 C15 1.364(10) . ?
C15 C16 1.392(8) . ?
C16 C160 1.503(8) . ?
C120 C121 1.521(11) . ?
C120 C122 1.524(10) . ?
C160 C161 1.487(10) . ?
C160 C162 1.525(10) . ?
