#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:53:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179311 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/08/4320821.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_4320821
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 Cr N6 O3 Si'
_chemical_formula_weight         464.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_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                 97.1566(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0132(6)
_cell_length_b                   13.7886(9)
_cell_length_c                   9.6481(7)
_cell_measurement_temperature    173(2)
_cell_volume                     1057.72(13)
_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 0.872
_diffrn_measured_fraction_theta_max 0.872
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5106
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.8841
_exptl_absorpt_correction_T_min  0.8581
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   DIFABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.524
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.524
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          1.228
_refine_ls_shift/su_mean         0.086
_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          0.1841
_refine_ls_wR_factor_ref         0.2041
_reflns_number_gt                1981
_reflns_number_total             2383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990945l_3.cif
_cod_data_source_block           drab09
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_database_code               4320821
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.44407(9) 0.2500 0.21694(7) 0.0182(3) Uani 1 2 d S . .
Si1 Si 0.45810(18) 0.2500 0.56939(14) 0.0240(4) Uani 1 2 d S . .
O1 O 0.5867(4) 0.1089(2) 0.0286(3) 0.0407(8) Uani 1 1 d . . .
O2 O 0.1733(6) 0.2500 -0.0247(4) 0.0460(13) Uani 1 2 d S . .
N1 N 0.3355(4) 0.1446(2) 0.3457(3) 0.0210(7) Uani 1 1 d . . .
N2 N 0.3546(4) 0.1481(3) 0.4906(3) 0.0238(7) Uani 1 1 d . . .
N3 N 0.6658(5) 0.2500 0.3732(4) 0.0226(9) Uani 1 2 d S . .
N4 N 0.6591(5) 0.2500 0.5162(4) 0.0235(10) Uani 1 2 d S . .
C1 C 0.1934(6) 0.0348(4) 0.1622(4) 0.0413(11) Uani 1 1 d . . .
H1A H 0.2357 0.0821 0.0993 0.062 Uiso 1 1 calc R . .
H1B H 0.0703 0.0326 0.1449 0.062 Uiso 1 1 calc R . .
H1C H 0.2390 -0.0295 0.1453 0.062 Uiso 1 1 calc R . .
C2 C 0.2470(5) 0.0639(3) 0.3106(4) 0.0294(9) Uani 1 1 d . . .
C3 C 0.2117(5) 0.0152(3) 0.4319(5) 0.0353(10) Uani 1 1 d . . .
H3A H 0.1511 -0.0438 0.4351 0.042 Uiso 1 1 calc R . .
C4 C 0.2804(5) 0.0684(3) 0.5434(4) 0.0301(9) Uani 1 1 d . . .
C5 C 0.2792(7) 0.0469(4) 0.6952(5) 0.0506(14) Uani 1 1 d . . .
H5A H 0.2171 -0.0134 0.7055 0.076 Uiso 1 1 calc R . .
H5B H 0.2246 0.1003 0.7392 0.076 Uiso 1 1 calc R . .
H5C H 0.3950 0.0396 0.7402 0.076 Uiso 1 1 calc R . .
C6 C 0.8948(8) 0.2500 0.2193(7) 0.0474(19) Uani 1 2 d S . .
H6A H 0.8020 0.2500 0.1461 0.071 Uiso 1 2 d SR . .
H6B H 0.9621 0.3069 0.2114 0.071 Uiso 0.50 1 d PR . .
C7 C 0.8290(6) 0.2500 0.3576(6) 0.0298(12) Uani 1 2 d S . .
C8 C 0.9259(7) 0.2500 0.4882(7) 0.0332(13) Uani 1 2 d S . .
H8A H 1.0465 0.2500 0.5051 0.040 Uiso 1 2 d SR . .
C9 C 0.8181(7) 0.2500 0.5873(6) 0.0316(13) Uani 1 2 d S . .
C10 C 0.8580(10) 0.2500 0.7431(7) 0.0503(19) Uani 1 2 d S . .
H10A H 0.7583 0.2500 0.7890 0.075 Uiso 1 2 d SR . .
H10B H 0.9233 0.1932 0.7699 0.075 Uiso 0.50 1 d PR . .
C11 C 0.4622(9) 0.2500 0.7581(6) 0.0437(17) Uani 1 2 d S . .
H11A H 0.5197 0.3069 0.7965 0.066 Uiso 0.50 1 d PR . .
H11B H 0.3490 0.2500 0.7810 0.066 Uiso 1 2 d SR . .
C12 C 0.5333(5) 0.1612(3) 0.1080(4) 0.0267(8) Uani 1 1 d . . .
C13 C 0.2713(6) 0.2500 0.0764(5) 0.0268(12) 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'
Cr Cr 0.3209 0.6236 '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
C13 Cr1 C12 83.47(17) . . ?
C13 Cr1 C12 83.47(17) . 4_565 ?
C12 Cr1 C12 84.7(3) . 4_565 ?
C13 Cr1 N1 96.03(14) . 4_565 ?
C12 Cr1 N1 179.46(15) . 4_565 ?
C12 Cr1 N1 95.45(15) 4_565 4_565 ?
C13 Cr1 N1 96.03(14) . . ?
C12 Cr1 N1 95.45(16) . . ?
C12 Cr1 N1 179.46(15) 4_565 . ?
N1 Cr1 N1 84.38(16) 4_565 . ?
C13 Cr1 N3 175.38(19) . . ?
C12 Cr1 N3 93.13(14) . . ?
C12 Cr1 N3 93.13(14) 4_565 . ?
N1 Cr1 N3 87.39(11) 4_565 . ?
N1 Cr1 N3 87.39(11) . . ?
N4 Si1 N2 105.99(13) . . ?
N4 Si1 N2 105.99(13) . 4_565 ?
N2 Si1 N2 106.3(2) . 4_565 ?
N4 Si1 C11 113.1(3) . . ?
N2 Si1 C11 112.48(15) . . ?
N2 Si1 C11 112.48(15) 4_565 . ?
C2 N1 N2 105.8(3) . . ?
C2 N1 Cr1 130.6(2) . . ?
N2 N1 Cr1 123.6(2) . . ?
C4 N2 N1 110.2(3) . . ?
C4 N2 Si1 132.9(3) . . ?
N1 N2 Si1 116.8(2) . . ?
C7 N3 N4 105.7(4) . . ?
C7 N3 Cr1 130.3(4) . . ?
N4 N3 Cr1 123.9(3) . . ?
C9 N4 N3 110.5(4) . . ?
C9 N4 Si1 133.2(4) . . ?
N3 N4 Si1 116.3(3) . . ?
N1 C2 C3 110.0(4) . . ?
N1 C2 C1 123.0(4) . . ?
C3 C2 C1 127.1(4) . . ?
C4 C3 C2 107.3(4) . . ?
C5 C4 C3 128.1(4) . . ?
C5 C4 N2 125.2(4) . . ?
C3 C4 N2 106.8(3) . . ?
N3 C7 C8 110.0(5) . . ?
N3 C7 C6 124.1(5) . . ?
C8 C7 C6 126.0(5) . . ?
C9 C8 C7 107.6(5) . . ?
C10 C9 N4 124.9(6) . . ?
C10 C9 C8 128.9(6) . . ?
N4 C9 C8 106.2(5) . . ?
O1 C12 Cr1 174.5(3) . . ?
O2 C13 Cr1 172.3(5) . . ?
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
Cr1 C13 1.813(5) . ?
Cr1 C12 1.817(4) . ?
Cr1 C12 1.817(4) 4_565 ?
Cr1 N1 2.164(3) 4_565 ?
Cr1 N1 2.164(3) . ?
Cr1 N3 2.182(4) . ?
Si1 N4 1.751(5) . ?
Si1 N2 1.755(3) . ?
Si1 N2 1.755(3) 4_565 ?
Si1 C11 1.817(6) . ?
O1 C12 1.172(5) . ?
O2 C13 1.173(7) . ?
N1 C2 1.340(5) . ?
N1 N2 1.389(4) . ?
N2 C4 1.378(5) . ?
N3 C7 1.335(6) . ?
N3 N4 1.387(6) . ?
N4 C9 1.370(7) . ?
C1 C2 1.498(5) . ?
C2 C3 1.408(6) . ?
C3 C4 1.361(6) . ?
C4 C5 1.495(6) . ?
C6 C7 1.495(8) . ?
C7 C8 1.395(8) . ?
C8 C9 1.366(9) . ?
C9 C10 1.497(9) . ?
