#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:34:13 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178657 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/68/4076876.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_4076876
loop_
_publ_author_name
'Bradley, Sam'
'Camm, Kenneth D.'
'Furtado, Stephen J.'
'Gott, Andrew L.'
'McGowan, Patrick C.'
'Podesta, Thomas J.'
'Thornton-Pett, Mark'
_publ_section_title
;
 Synthesis and Structure of Amino-Functionalized Cyclopentadienyl Vanadium
 Complexes and Evaluation of Their Butadiene Polymerization Behavior
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3443
_journal_paper_doi               10.1021/om020170f
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C11 H16 Cl2 Cr N'
_chemical_formula_weight         285.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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
_cell_angle_beta                 98.0140(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.89940(10)
_cell_length_b                   12.6044(2)
_cell_length_c                   12.0900(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1192.01(4)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection
'DENZO-SMN and COLLECT (Otwinowski & Minor, 1996)'
_computing_data_reduction
'DENZO-SMN and COLLECT (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    ORTEX
_computing_publication_material  'WinCIF (Thornton-Pett, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius KappaCCD area-detector diffractometer'
_diffrn_radiation_detector       'CCD plate'
_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  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22221
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.7166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
?
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.0055(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     Shelxl
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0358P)²+0.4651P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                2151
_reflns_number_total             2348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020170f.cif
_cod_data_source_block           kccr
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4076876
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 0.2759(2) -0.15514(13) 0.80715(15) 0.0279(4) Uani 1 1 d
C2 C 0.3382(3) -0.10813(15) 0.91153(16) 0.0342(4) Uani 1 1 d
H2 H 0.4539 -0.09 0.9369 0.041 Uiso 1 1 calc
C3 C 0.1984(3) -0.09287(15) 0.97134(16) 0.0408(5) Uani 1 1 d
H3 H 0.2044 -0.0632 1.044 0.049 Uiso 1 1 calc
C4 C 0.0502(3) -0.12880(15) 0.90541(17) 0.0392(5) Uani 1 1 d
H4 H -0.0619 -0.1279 0.9255 0.047 Uiso 1 1 calc
C5 C 0.0961(2) -0.16697(13) 0.80300(16) 0.0316(4) Uani 1 1 d
H5 H 0.02 -0.1954 0.7424 0.038 Uiso 1 1 calc
C6 C 0.3776(2) -0.17595(14) 0.71280(16) 0.0321(4) Uani 1 1 d
H6 H 0.4232 -0.25 0.7202 0.039 Uiso 1 1 calc
C7 C 0.5285(2) -0.09939(15) 0.71611(18) 0.0365(4) Uani 1 1 d
H7A H 0.6044 -0.1236 0.6625 0.044 Uiso 1 1 calc
H7B H 0.5953 -0.1004 0.7918 0.044 Uiso 1 1 calc
C8 C 0.4697(2) 0.01456(14) 0.68695(17) 0.0305(4) Uani 1 1 d
H8A H 0.5156 0.062 0.7493 0.037 Uiso 1 1 calc
H8B H 0.5186 0.0376 0.6198 0.037 Uiso 1 1 calc
C9 C 0.2417(2) 0.13546(14) 0.62059(15) 0.0308(4) Uani 1 1 d
H9A H 0.1176 0.1458 0.6057 0.037 Uiso 1 1 calc
H9B H 0.2909 0.1443 0.5511 0.037 Uiso 1 1 calc
H9C H 0.2917 0.1879 0.6755 0.037 Uiso 1 1 calc
C10 C 0.2069(2) -0.05028(15) 0.57661(15) 0.0340(4) Uani 1 1 d
H10A H 0.239 -0.0271 0.5041 0.041 Uiso 1 1 calc
H10B H 0.0806 -0.0486 0.5701 0.041 Uiso 1 1 calc
C11 C 0.2680(3) -0.16501(15) 0.59925(16) 0.0390(5) Uani 1 1 d
H11A H 0.1675 -0.2123 0.5963 0.047 Uiso 1 1 calc
H11B H 0.3352 -0.1877 0.5401 0.047 Uiso 1 1 calc
N9 N 0.27929(18) 0.02686(11) 0.66527(11) 0.0238(3) Uani 1 1 d
Cl1 Cl 0.26607(5) 0.15790(3) 0.90069(3) 0.02919(13) Uani 1 1 d
Cl2 Cl -0.10432(5) 0.06342(3) 0.73736(3) 0.02865(13) Uani 1 1 d
Cr1 Cr 0.16159(3) 0.003737(18) 0.81337(2) 0.02035(11) Uani 1 1 d
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 0 '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'
Cl Cl 0.1484 0.1585 '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
C2 C1 C5 107.22(16)
C2 C1 C6 126.21(17)
C5 C1 C6 126.17(17)
C2 C1 Cr1 71.52(10)
C5 C1 Cr1 71.59(9)
C6 C1 Cr1 116.66(12)
C3 C2 C1 108.22(17)
C3 C2 Cr1 73.04(10)
C1 C2 Cr1 70.97(9)
C4 C3 C2 108.44(17)
C4 C3 Cr1 72.07(10)
C2 C3 Cr1 69.97(10)
C3 C4 C5 108.14(17)
C3 C4 Cr1 71.78(11)
C5 C4 Cr1 69.89(10)
C4 C5 C1 107.97(17)
C4 C5 Cr1 73.00(10)
C1 C5 Cr1 70.82(9)
C1 C6 C11 111.74(15)
C1 C6 C7 111.46(15)
C11 C6 C7 108.01(17)
C6 C7 C8 112.00(15)
N9 C8 C7 113.64(14)
N9 C10 C11 113.80(15)
C6 C11 C10 111.75(15)
C9 N9 C8 107.69(13)
C9 N9 C10 107.47(14)
C8 N9 C10 109.35(14)
C9 N9 Cr1 109.86(10)
C8 N9 Cr1 112.37(11)
C10 N9 Cr1 109.95(11)
N9 Cr1 C1 82.40(6)
N9 Cr1 C2 102.70(6)
C1 Cr1 C2 37.51(7)
N9 Cr1 C5 102.10(6)
C1 Cr1 C5 37.59(6)
C2 Cr1 C5 62.29(7)
N9 Cr1 C3 139.55(7)
C1 Cr1 C3 62.07(7)
C2 Cr1 C3 36.99(8)
C5 Cr1 C3 61.52(7)
N9 Cr1 C4 139.12(7)
C1 Cr1 C4 62.16(7)
C2 Cr1 C4 61.48(8)
C5 Cr1 C4 37.11(7)
C3 Cr1 C4 36.15(8)
N9 Cr1 Cl2 95.73(4)
C1 Cr1 Cl2 129.81(5)
C2 Cr1 Cl2 153.77(6)
C5 Cr1 Cl2 95.86(5)
C3 Cr1 Cl2 121.29(6)
C4 Cr1 Cl2 92.41(6)
N9 Cr1 Cl1 95.64(4)
C1 Cr1 Cl1 131.21(5)
C2 Cr1 Cl1 97.63(5)
C5 Cr1 Cl1 155.57(5)
C3 Cr1 Cl1 94.11(6)
C4 Cr1 Cl1 122.52(6)
Cl2 Cr1 Cl1 98.968(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.419(3)
C1 C5 1.423(2)
C1 C6 1.507(3)
C1 Cr1 2.2024(16)
C2 C3 1.415(3)
C2 Cr1 2.2095(17)
C3 C4 1.397(3)
C3 Cr1 2.2494(18)
C4 C5 1.422(3)
C4 Cr1 2.2531(18)
C5 Cr1 2.2124(17)
C6 C11 1.524(3)
C6 C7 1.530(3)
C7 C8 1.535(2)
C8 N9 1.499(2)
C9 N9 1.486(2)
C10 N9 1.500(2)
C10 C11 1.537(3)
N9 Cr1 2.1493(14)
Cl1 Cr1 2.3084(5)
Cl2 Cr1 2.2988(4)
