#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:53:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179311 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/08/4320819.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_4320819
loop_
_publ_author_name
'Eric E. Pullen'
'Daniel Rabinovich'
'Christopher D. Incarvito'
'Thomas E. Concolino'
'Arnold L. Rheingold'
_publ_contact_author
;
     Dr. Daniel Rabinovich
     Department of Chemistry
     The University of North Carolina at Charlotte
     9201 University City Boulevard
     Charlotte, NC 28223
     USA
;
_publ_contact_author_email       DRabinov@email.uncc.edu
_publ_contact_author_fax         +704-547-3151
_publ_contact_author_phone       +704-547-4442
_publ_section_title
;
 Syntheses and Structures of Methyltris(pyrazolyl)silane Complexes of the
 Group 6 Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1561
_journal_page_last               1567
_journal_paper_doi               10.1021/ic990945l
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C19 H24 N6 O3 Si W'
_chemical_formula_weight         596.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5761(2)
_cell_length_b                   14.1731(2)
_cell_length_c                   8.4049(2)
_cell_measurement_temperature    173(2)
_cell_volume                     2212.85(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9511
_diffrn_reflns_theta_full        28.43
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    5.307
_exptl_absorpt_correction_T_max  0.4166
_exptl_absorpt_correction_T_min  0.3505
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.109
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                2478
_reflns_number_total             2669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990945l_1.cif
_cod_data_source_block           drab07
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2212.85(4)
_cod_database_code               4320819
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.865336(13) 0.7500 -0.04479(2) 0.01935(14) Uani 1 2 d S . .
Si1 Si 0.67461(10) 0.7500 -0.0703(2) 0.0229(4) Uani 1 2 d S . .
O1 O 0.9776(2) 0.8953(3) -0.1714(5) 0.0482(10) Uani 1 1 d . . .
O2 O 0.9823(3) 0.7500 0.2212(6) 0.0513(16) Uani 1 2 d S . .
C1 C 0.8683(3) 0.9726(5) 0.1751(12) 0.060(2) Uani 1 1 d . . .
H1A H 0.9046 0.9293 0.1323 0.090 Uiso 1 1 calc R . .
H1B H 0.8728 0.9755 0.2911 0.090 Uiso 1 1 calc R . .
H1C H 0.8758 1.0357 0.1302 0.090 Uiso 1 1 calc R . .
C2 C 0.7942(3) 0.9377(3) 0.1311(6) 0.0380(11) Uani 1 1 d . . .
C3 C 0.7267(4) 0.9798(4) 0.1683(7) 0.0495(15) Uani 1 1 d . . .
H3A H 0.7194 1.0364 0.2266 0.059 Uiso 1 1 calc R . .
C4 C 0.6747(3) 0.9238(4) 0.1047(7) 0.0376(12) Uani 1 1 d . . .
C5 C 0.5940(4) 0.9359(6) 0.1117(10) 0.064(2) Uani 1 1 d . . .
H5A H 0.5824 0.9944 0.1681 0.096 Uiso 1 1 calc R . .
H5B H 0.5727 0.8822 0.1682 0.096 Uiso 1 1 calc R . .
H5C H 0.5746 0.9387 0.0034 0.096 Uiso 1 1 calc R . .
C6 C 0.8860(5) 0.7500 -0.4705(9) 0.074(5) Uani 1 2 d S . .
H6A H 0.9179 0.7500 -0.3777 0.110 Uiso 1 2 d SR . .
H6B H 0.8952 0.8065 -0.5347 0.110 Uiso 0.50 1 d PR . .
C7 C 0.8090(4) 0.7500 -0.4158(8) 0.0324(15) Uani 1 2 d S . .
C8 C 0.7479(4) 0.7500 -0.5120(8) 0.0340(15) Uani 1 2 d S . .
H8A H 0.7471 0.7500 -0.6251 0.041 Uiso 1 2 calc SR . .
C9 C 0.6888(4) 0.7500 -0.4134(8) 0.0332(15) Uani 1 2 d S . .
C10 C 0.6107(6) 0.7500 -0.4582(8) 0.052(3) Uani 1 2 d S . .
H10A H 0.6063 0.7500 -0.5744 0.078 Uiso 1 2 d SR . .
H10B H 0.5873 0.8065 -0.4149 0.078 Uiso 0.50 1 d PR . .
C11 C 0.5765(4) 0.7500 -0.0878(10) 0.0378(17) Uani 1 2 d S . .
H11A H 0.5552 0.7500 0.0189 0.057 Uiso 1 2 d SR . .
H11B H 0.5608 0.6935 -0.1455 0.057 Uiso 0.50 1 d PR . .
C12 C 0.9328(3) 0.8430(3) -0.1256(5) 0.0305(9) Uani 1 1 d . . .
C13 C 0.9336(4) 0.7500 0.1302(7) 0.0308(14) Uani 1 2 d S . .
N1 N 0.7836(2) 0.8571(3) 0.0496(4) 0.0249(8) Uani 1 1 d . . .
N2 N 0.7075(2) 0.8484(3) 0.0331(4) 0.0256(8) Uani 1 1 d . . .
N3 N 0.7917(3) 0.7500 -0.2619(6) 0.0222(10) Uani 1 2 d S . .
N4 N 0.7156(3) 0.7500 -0.2585(6) 0.0237(10) Uani 1 2 d S . .
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
C12 W1 C12 85.5(3) . 7_575 ?
C12 W1 C13 81.00(19) . . ?
C12 W1 C13 81.00(19) 7_575 . ?
C12 W1 N3 96.14(17) . . ?
C12 W1 N3 96.14(17) 7_575 . ?
C13 W1 N3 176.1(2) . . ?
C12 W1 N1 178.62(17) . 7_575 ?
C12 W1 N1 95.69(18) 7_575 7_575 ?
C13 W1 N1 99.82(17) . 7_575 ?
N3 W1 N1 83.08(13) . 7_575 ?
C12 W1 N1 95.69(18) . . ?
C12 W1 N1 178.62(17) 7_575 . ?
C13 W1 N1 99.82(17) . . ?
N3 W1 N1 83.08(13) . . ?
N1 W1 N1 83.1(2) 7_575 . ?
N2 Si1 N2 105.4(3) 7_575 . ?
N2 Si1 N4 107.16(16) 7_575 . ?
N2 Si1 N4 107.16(16) . . ?
N2 Si1 C11 112.8(2) 7_575 . ?
N2 Si1 C11 112.8(2) . . ?
N4 Si1 C11 111.1(3) . . ?
N1 C2 C3 109.9(5) . . ?
N1 C2 C1 122.3(5) . . ?
C3 C2 C1 127.8(5) . . ?
C4 C3 C2 107.2(4) . . ?
C3 C4 N2 108.2(5) . . ?
C3 C4 C5 128.6(5) . . ?
N2 C4 C5 123.2(5) . . ?
N3 C7 C8 111.5(6) . . ?
N3 C7 C6 121.8(6) . . ?
C8 C7 C6 126.7(6) . . ?
C9 C8 C7 107.5(6) . . ?
C8 C9 N4 106.1(6) . . ?
C8 C9 C10 128.4(7) . . ?
N4 C9 C10 125.5(6) . . ?
O1 C12 W1 175.3(4) . . ?
O2 C13 W1 171.0(5) . . ?
C2 N1 N2 105.5(4) . . ?
C2 N1 W1 130.0(4) . . ?
N2 N1 W1 124.5(3) . . ?
C4 N2 N1 109.3(4) . . ?
C4 N2 Si1 133.1(4) . . ?
N1 N2 Si1 117.6(3) . . ?
C7 N3 N4 105.1(5) . . ?
C7 N3 W1 129.2(5) . . ?
N4 N3 W1 125.7(3) . . ?
C9 N4 N3 109.8(5) . . ?
C9 N4 Si1 133.3(5) . . ?
N3 N4 Si1 116.8(4) . . ?
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
W1 C12 1.941(5) . ?
W1 C12 1.941(5) 7_575 ?
W1 C13 1.942(6) . ?
W1 N3 2.280(5) . ?
W1 N1 2.288(4) 7_575 ?
W1 N1 2.288(4) . ?
Si1 N2 1.752(4) 7_575 ?
Si1 N2 1.752(4) . ?
Si1 N4 1.757(5) . ?
Si1 C11 1.829(8) . ?
O1 C12 1.179(6) . ?
O2 C13 1.184(8) . ?
C1 C2 1.510(8) . ?
C2 N1 1.347(6) . ?
C2 C3 1.422(8) . ?
C3 C4 1.360(9) . ?
C4 N2 1.370(6) . ?
C4 C5 1.509(10) . ?
C6 C7 1.502(10) . ?
C7 N3 1.334(8) . ?
C7 C8 1.395(10) . ?
C8 C9 1.375(10) . ?
C9 N4 1.394(9) . ?
C9 C10 1.500(11) . ?
N1 N2 1.426(6) . ?
N3 N4 1.413(7) . ?
