#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/20/7012057.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_7012057
loop_
_publ_author_name
'Thomas Rüther'
'Kingsley J. Cavell'
'Nathalie C. Braussaud'
'Brian W. Skelton'
'Allan H. White'
_publ_section_title
;
 Synthesis, characterisation and catalytic behaviour of a novel class
 of chromium(III) and vanadium(III) complexes containing bi- and
 tri-dentate imidazole chelating ligands: a comparative study
;
_journal_issue                   24
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4684
_journal_page_last               4693
_journal_paper_doi               10.1039/b207248c
_journal_year                    2002
_chemical_formula_sum            'C13 H16 Cl3 Cr N6 O'
_chemical_formula_weight         430.67
_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'
_audit_creation_date             01-02-13
_audit_creation_method           Xtal3.6
_cell_angle_alpha                90.00000
_cell_angle_beta                 94.4190(10)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   6.9757(2)
_cell_length_b                   14.6946(5)
_cell_length_c                   17.5803(6)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      2.6
_cell_volume                     1796.71(10)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .024
_diffrn_reflns_av_sigmaI/netI    .071
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37346
_diffrn_reflns_theta_max         37.61
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  .83
_exptl_absorpt_correction_T_min  .72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       bar
_exptl_crystal_F_000             876
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .1
_refine_diff_density_max         .547
_refine_diff_density_min         -.373
_refine_ls_goodness_of_fit_all   .983
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     281
_refine_ls_number_reflns         6992
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .051
_refine_ls_R_factor_gt           .03
_refine_ls_shift/su_max          .022
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .038
_refine_ls_wR_factor_ref         .035
_reflns_d_resolution_high        .582
_reflns_d_resolution_low         11.236
_reflns_Friedel_coverage         0
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              -30
_reflns_number_gt                6992
_reflns_number_total             9433
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            b207248c.txt
_cod_data_source_block           trcr
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_sg_symbol_H-M      P_1_21/n_1
_cod_original_formula_sum        'C13 H16 Cl3 Cr1 N6 O1'
_cod_database_code               7012057
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr .72277(2) .745190(11) .050928(9) .01385(7) Uani ? ? 1.00000 ? ?
Cl1 .87174(4) .793591(18) -.056055(15) .01997(11) Uani ? ? 1.00000 ? ?
Cl2 .53935(4) .638728(18) -.019714(15) .01817(11) Uani ? ? 1.00000 ? ?
Cl3 .89998(5) .84631(2) .128404(17) .02453(13) Uani ? ? 1.00000 ? ?
N11 .58213(13) .70568(6) .14453(5) .0171(4) Uani ? ? 1.00000 ? ?
C12 .58655(15) .62238(7) .17538(6) .0161(4) Uani ? ? 1.00000 ? ?
N13 .46729(14) .61854(7) .23269(5) .0191(4) Uani ? ? 1.00000 ? ?
C14 .38439(18) .70257(9) .23799(7) .0246(5) Uani ? ? 1.00000 ? ?
C15 .45545(19) .75569(8) .18293(7) .0232(5) Uani ? ? 1.00000 ? ?
C16 .4399(2) .54234(9) .28504(7) .0258(6) Uani ? ? 1.00000 ? ?
C0 .70584(15) .54505(7) .15408(6) .0166(4) Uani ? ? 1.00000 ? ?
O0 .66796(13) .46757(6) .17223(5) .0247(4) Uani ? ? 1.00000 ? ?
N21 .91627(13) .64434(6) .07901(5) .0152(4) Uani ? ? 1.00000 ? ?
C22 .87957(15) .56644(7) .11493(6) .0154(4) Uani ? ? 1.00000 ? ?
N23 1.03057(13) .50863(6) .11259(5) .0174(4) Uani ? ? 1.00000 ? ?
C24 1.16747(16) .55135(8) .07390(7) .0194(5) Uani ? ? 1.00000 ? ?
C25 1.09581(15) .63514(8) .05325(6) .0181(4) Uani ? ? 1.00000 ? ?
C26 1.0518(2) .41760(8) .14647(8) .0268(6) Uani ? ? 1.00000 ? ?
N101 .50873(14) .84106(6) .02770(6) .0198(4) Uani ? ? 1.00000 ? ?
C101 .38891(16) .89290(7) .01770(7) .0198(5) Uani ? ? 1.00000 ? ?
C102 .23451(19) .95930(9) .00617(9) .0276(6) Uani ? ? 1.00000 ? ?
N201 .9699(2) .55825(12) .31958(9) .0490(8) Uani ? ? 1.00000 ? ?
C201 .9280(2) .63345(12) .32054(8) .0362(7) Uani ? ? 1.00000 ? ?
C202 .8740(3) .72886(14) .32181(11) .0467(10) Uani ? ? 1.00000 ? ?
H14 .297(2) .7154(10) .2758(9) .024(4) Uiso ? ? 1.00000 ? ?
H15 .429(2) .8176(10) .1697(8) .022(4) Uiso ? ? 1.00000 ? ?
H16a .564(2) .5158(10) .3011(9) .024(4) Uiso ? ? 1.00000 ? ?
H16b .366(3) .5000(13) .2608(11) .044(5) Uiso ? ? 1.00000 ? ?
H16c .378(2) .5665(12) .3278(10) .040(5) Uiso ? ? 1.00000 ? ?
H24 1.278(2) .5243(11) .0683(9) .031(4) Uiso ? ? 1.00000 ? ?
H25 1.153(2) .6785(10) .0255(9) .022(4) Uiso ? ? 1.00000 ? ?
H26a 1.031(2) .4221(11) .1970(9) .032(4) Uiso ? ? 1.00000 ? ?
H26b 1.179(2) .3983(11) .1412(9) .034(4) Uiso ? ? 1.00000 ? ?
H26c .968(2) .3782(12) .1185(10) .037(5) Uiso ? ? 1.00000 ? ?
H102a .233(3) .9846(13) -.0407(11) .047(5) Uiso ? ? 1.00000 ? ?
H102b .253(2) 1.0045(12) .0442(10) .036(5) Uiso ? ? 1.00000 ? ?
H102c .120(3) .9277(13) .0119(11) .053(6) Uiso ? ? 1.00000 ? ?
H202a .749(4) .7340(15) .3327(13) .073(8) Uiso ? ? 1.00000 ? ?
H202b .869(3) .7539(15) .2699(15) .074(7) Uiso ? ? 1.00000 ? ?
H202c .958(3) .7616(13) .3541(12) .053(6) Uiso ? ? 1.00000 ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 52 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 64 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Cl ? 0 12 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Cr ? 0 4 .284 .624 'Int Tables Vol IV Tables 2.2B and 2.3.1'
N ? 0 24 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 4 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Cr Cl2 . . . 92.041(11) ?
Cl1 Cr Cl3 . . . 91.601(12) ?
Cl1 Cr N11 . . . 177.79(4) ?
Cl1 Cr N21 . . . 95.12(3) ?
Cl1 Cr N101 . . . 89.59(3) ?
Cl2 Cr Cl3 . . . 176.232(17) ?
Cl2 Cr N11 . . . 87.75(3) ?
Cl2 Cr N21 . . . 88.11(3) ?
Cl2 Cr N101 . . . 89.64(3) ?
Cl3 Cr N11 . . . 88.65(3) ?
Cl3 Cr N21 . . . 90.60(3) ?
Cl3 Cr N101 . . . 91.35(3) ?
N11 Cr N21 . . . 87.07(4) ?
N11 Cr N101 . . . 88.21(4) ?
N21 Cr N101 . . . 174.85(4) ?
Cr N11 C12 . . . 125.67(7) ?
Cr N11 C15 . . . 127.44(8) ?
C12 N11 C15 . . . 106.69(9) ?
N11 C12 N13 . . . 110.05(9) ?
N11 C12 C0 . . . 126.74(10) ?
N13 C12 C0 . . . 123.18(10) ?
C12 N13 C14 . . . 107.42(10) ?
C12 N13 C16 . . . 127.82(10) ?
C14 N13 C16 . . . 124.59(10) ?
N13 C14 C15 . . . 106.79(11) ?
N13 C14 H14 . . . 121.4(9) ?
C15 C14 H14 . . . 131.8(9) ?
N11 C15 C14 . . . 109.05(11) ?
N11 C15 H15 . . . 120.9(9) ?
C14 C15 H15 . . . 130.0(9) ?
N13 C16 H16a . . . 109.3(9) ?
N13 C16 H16b . . . 109.2(12) ?
N13 C16 H16c . . . 107.2(10) ?
H16a C16 H16b . . . 109.0(15) ?
H16a C16 H16c . . . 111.4(14) ?
H16b C16 H16c . . . 110.6(16) ?
C12 C0 O0 . . . 121.10(10) ?
C12 C0 C22 . . . 117.07(9) ?
O0 C0 C22 . . . 121.69(10) ?
Cr N21 C22 . . . 125.96(7) ?
Cr N21 C25 . . . 126.59(7) ?
C22 N21 C25 . . . 106.48(9) ?
C0 C22 N21 . . . 126.57(9) ?
C0 C22 N23 . . . 123.32(9) ?
N21 C22 N23 . . . 110.08(9) ?
C22 N23 C24 . . . 107.54(9) ?
C22 N23 C26 . . . 127.81(10) ?
C24 N23 C26 . . . 124.63(10) ?
N23 C24 C25 . . . 106.88(10) ?
N23 C24 H24 . . . 120.1(10) ?
C25 C24 H24 . . . 133.0(10) ?
N21 C25 C24 . . . 109.01(10) ?
N21 C25 H25 . . . 123.7(9) ?
C24 C25 H25 . . . 127.2(9) ?
N23 C26 H26a . . . 108.0(11) ?
N23 C26 H26b . . . 107.5(10) ?
N23 C26 H26c . . . 108.2(11) ?
H26a C26 H26b . . . 109.7(14) ?
H26a C26 H26c . . . 114.7(15) ?
H26b C26 H26c . . . 108.5(15) ?
Cr N101 C101 . . . 177.31(10) ?
N101 C101 C102 . . . 179.06(15) ?
C101 C102 H102a . . . 110.9(12) ?
C101 C102 H102b . . . 108.1(10) ?
C101 C102 H102c . . . 106.4(12) ?
H102a C102 H102b . . . 110.3(16) ?
H102a C102 H102c . . . 110.8(16) ?
H102b C102 H102c . . . 110.2(16) ?
N201 C201 C202 . . . 179.7(2) ?
C201 C202 H202a . . . 109.7(14) ?
C201 C202 H202b . . . 109.8(13) ?
C201 C202 H202c . . . 111.1(12) ?
H202a C202 H202b . . . 102(2) ?
H202a C202 H202c . . . 114(2) ?
H202b C202 H202c . . . 110.5(19) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cr Cl1 . . 2.3290(3) ?
Cr Cl2 . . 2.3199(3) ?
Cr Cl3 . . 2.3090(3) ?
Cr N11 . . 2.0630(10) ?
Cr N21 . . 2.0394(9) ?
Cr N101 . . 2.0704(10) ?
N11 C12 . . 1.3382(14) ?
N11 C15 . . 1.3670(16) ?
C12 N13 . . 1.3563(15) ?
C12 C0 . . 1.4738(15) ?
N13 C14 . . 1.3697(16) ?
N13 C16 . . 1.4713(17) ?
C14 C15 . . 1.3660(18) ?
C14 H14 . . .954(16) ?
C15 H15 . . .954(14) ?
C16 H16a . . .972(15) ?
C16 H16b . . .894(18) ?
C16 H16c . . .963(18) ?
C0 O0 . . 1.2169(13) ?
C0 C22 . . 1.4730(15) ?
N21 C22 . . 1.3414(13) ?
N21 C25 . . 1.3709(14) ?
C22 N23 . . 1.3563(14) ?
N23 C24 . . 1.3671(15) ?
N23 C26 . . 1.4672(16) ?
C24 C25 . . 1.3673(16) ?
C24 H24 . . .882(16) ?
C25 H25 . . .912(15) ?
C26 H26a . . .913(17) ?
C26 H26b . . .942(17) ?
C26 H26c . . .936(17) ?
N101 C101 . . 1.1346(15) ?
C101 C102 . . 1.4558(17) ?
C102 H102a . . .90(2) ?
C102 H102b . . .944(17) ?
C102 H102c . . .94(2) ?
N201 C201 . . 1.143(2) ?
C201 C202 . . 1.453(3) ?
C202 H202a . . .91(3) ?
C202 H202b . . .98(3) ?
C202 H202c . . .92(2) ?
