#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:47:51 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179263 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/83/4318388.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_4318388
loop_
_publ_author_name
'Kunal K. Kamar'
'Amrita Saha'
'Alfonso Castiñeiras'
'Chen-Hsiung Hung'
'Sreebrata Goswami'
_publ_section_title
;
 Chromium Complexes of an Isomeric N-Donor Ligand,
 2-[(N-Arylamino)phenylazo]pyridine: Amination Reactions, X-ray Structure,
 and Redox Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4531
_journal_page_last               4538
_journal_paper_doi               10.1021/ic0201497
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C34 H26 Cl Cr N8 O4'
_chemical_formula_weight         698.08
_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                103.975(3)
_cell_angle_beta                 91.119(3)
_cell_angle_gamma                93.829(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1815(12)
_cell_length_b                   10.3470(14)
_cell_length_c                   17.220(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1582.9(4)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.2835
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10266
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.8245
_exptl_absorpt_correction_type   'Empirical Used SADABS'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Thin Plate'
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.607
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.607
_refine_ls_R_factor_all          0.1685
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0528P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                1922
_reflns_number_total             7069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0201497_1.cif
_cod_data_source_block           C34H26ClCrN8O4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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               4318388
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.50271(8) 0.80994(7) 0.73097(4) 0.0335(2) Uani 1 1 d . . .
N1 N 0.3193(4) 0.8023(4) 0.7803(2) 0.0463(10) Uani 1 1 d . . .
N2 N 0.4142(4) 0.9324(4) 0.6857(2) 0.0483(11) Uani 1 1 d . . .
N3 N 0.4786(5) 0.9889(4) 0.6339(2) 0.0577(12) Uani 1 1 d . . .
N4 N 0.6508(4) 0.8422(4) 0.6571(2) 0.0509(11) Uani 1 1 d . . .
C1 C 0.2643(5) 0.7042(5) 0.8209(3) 0.0493(13) Uani 1 1 d . . .
C2 C 0.3127(6) 0.7111(6) 0.8983(3) 0.0619(15) Uani 1 1 d . . .
H2 H 0.3810 0.7791 0.9241 0.074 Uiso 1 1 calc R . .
C3 C 0.2595(7) 0.6169(7) 0.9374(4) 0.082(2) Uani 1 1 d . . .
H3 H 0.2911 0.6226 0.9899 0.099 Uiso 1 1 calc R . .
C4 C 0.1609(8) 0.5157(7) 0.8998(5) 0.093(2) Uani 1 1 d . . .
H4 H 0.1248 0.4529 0.9265 0.111 Uiso 1 1 calc R . .
C5 C 0.1157(7) 0.5071(6) 0.8229(5) 0.091(2) Uani 1 1 d . . .
H5 H 0.0502 0.4368 0.7970 0.109 Uiso 1 1 calc R . .
C6 C 0.1657(6) 0.6017(6) 0.7824(3) 0.0682(16) Uani 1 1 d . . .
H6 H 0.1329 0.5957 0.7301 0.082 Uiso 1 1 calc R . .
C7 C 0.2276(6) 0.8900(5) 0.7650(3) 0.0491(13) Uani 1 1 d . . .
C8 C 0.0897(6) 0.9156(5) 0.7978(3) 0.0592(15) Uani 1 1 d . . .
H8 H 0.0498 0.8642 0.8307 0.071 Uiso 1 1 calc R . .
C9 C 0.0157(6) 1.0154(6) 0.7812(3) 0.0729(17) Uani 1 1 d . . .
H9 H -0.0740 1.0324 0.8043 0.087 Uiso 1 1 calc R . .
C10 C 0.0689(6) 1.0936(6) 0.7308(4) 0.0729(17) Uani 1 1 d . . .
H10 H 0.0147 1.1611 0.7210 0.087 Uiso 1 1 calc R . .
C11 C 0.2001(6) 1.0717(5) 0.6959(3) 0.0631(15) Uani 1 1 d . . .
H11 H 0.2356 1.1222 0.6615 0.076 Uiso 1 1 calc R . .
C12 C 0.2793(6) 0.9705(5) 0.7134(3) 0.0509(13) Uani 1 1 d . . .
C13 C 0.6125(6) 0.9359(5) 0.6177(3) 0.0554(14) Uani 1 1 d . . .
C14 C 0.7039(7) 0.9773(6) 0.5634(3) 0.0753(18) Uani 1 1 d . . .
H14 H 0.6788 1.0429 0.5381 0.090 Uiso 1 1 calc R . .
C15 C 0.8334(7) 0.9166(7) 0.5488(4) 0.084(2) Uani 1 1 d . . .
H15 H 0.8955 0.9408 0.5119 0.100 Uiso 1 1 calc R . .
C16 C 0.8738(7) 0.8207(7) 0.5875(4) 0.080(2) Uani 1 1 d . . .
H16 H 0.9618 0.7812 0.5773 0.095 Uiso 1 1 calc R . .
C17 C 0.7805(6) 0.7861(5) 0.6409(3) 0.0606(15) Uani 1 1 d . . .
H17 H 0.8062 0.7220 0.6673 0.073 Uiso 1 1 calc R . .
N5 N 0.5956(4) 0.9404(4) 0.8198(2) 0.0453(10) Uani 1 1 d . . .
N6 N 0.6025(4) 0.6929(4) 0.7765(2) 0.0447(11) Uani 1 1 d . . .
N7 N 0.5958(4) 0.5645(4) 0.7457(2) 0.0525(11) Uani 1 1 d . . .
N8 N 0.4437(4) 0.6381(4) 0.6566(2) 0.0482(11) Uani 1 1 d . . .
C18 C 0.5719(5) 1.0795(5) 0.8402(3) 0.0471(13) Uani 1 1 d . . .
C19 C 0.4700(6) 1.1283(5) 0.8948(3) 0.0668(16) Uani 1 1 d . . .
H19 H 0.4204 1.0717 0.9215 0.080 Uiso 1 1 calc R . .
C20 C 0.4409(6) 1.2611(6) 0.9103(4) 0.0814(19) Uani 1 1 d . . .
H20 H 0.3714 1.2934 0.9472 0.098 Uiso 1 1 calc R . .
C21 C 0.5139(6) 1.3454(6) 0.8717(3) 0.0728(18) Uani 1 1 d . . .
H21 H 0.4932 1.4345 0.8817 0.087 Uiso 1 1 calc R . .
C22 C 0.6174(6) 1.2983(5) 0.8182(3) 0.0611(15) Uani 1 1 d . . .
H22 H 0.6687 1.3558 0.7928 0.073 Uiso 1 1 calc R . .
C23 C 0.6458(5) 1.1655(5) 0.8021(3) 0.0514(14) Uani 1 1 d . . .
H23 H 0.7153 1.1336 0.7651 0.062 Uiso 1 1 calc R . .
C24 C 0.6809(5) 0.8868(5) 0.8679(3) 0.0416(12) Uani 1 1 d . . .
C25 C 0.7598(5) 0.9575(5) 0.9385(3) 0.0535(14) Uani 1 1 d . . .
H25 H 0.7545 1.0491 0.9578 0.064 Uiso 1 1 calc R . .
C26 C 0.8446(5) 0.8871(6) 0.9778(3) 0.0608(16) Uani 1 1 d . . .
H26 H 0.8951 0.9332 1.0247 0.073 Uiso 1 1 calc R . .
C27 C 0.8590(6) 0.7506(6) 0.9513(3) 0.0658(16) Uani 1 1 d . . .
H27 H 0.9208 0.7079 0.9788 0.079 Uiso 1 1 calc R . .
C28 C 0.7816(5) 0.6807(5) 0.8847(3) 0.0555(14) Uani 1 1 d . . .
H28 H 0.7890 0.5893 0.8662 0.067 Uiso 1 1 calc R . .
C29 C 0.6906(5) 0.7480(5) 0.8444(3) 0.0429(12) Uani 1 1 d . . .
C30 C 0.5039(6) 0.5349(5) 0.6781(3) 0.0517(14) Uani 1 1 d . . .
C31 C 0.4748(6) 0.4039(5) 0.6345(3) 0.0668(16) Uani 1 1 d . . .
H31 H 0.5181 0.3343 0.6493 0.080 Uiso 1 1 calc R . .
C32 C 0.3807(7) 0.3795(6) 0.5690(4) 0.0782(19) Uani 1 1 d . . .
H32 H 0.3594 0.2925 0.5389 0.094 Uiso 1 1 calc R . .
C33 C 0.3176(6) 0.4834(6) 0.5475(3) 0.0720(17) Uani 1 1 d . . .
H33 H 0.2526 0.4670 0.5036 0.086 Uiso 1 1 calc R . .
C34 C 0.3520(5) 0.6121(5) 0.5920(3) 0.0605(15) Uani 1 1 d . . .
H34 H 0.3108 0.6825 0.5769 0.073 Uiso 1 1 calc R . .
Cl1 Cl 0.89857(19) 0.34286(18) 0.60630(10) 0.0774(5) Uani 1 1 d . . .
O1 O 0.8967(6) 0.4823(5) 0.6164(3) 0.145(2) Uani 1 1 d . . .
O2 O 0.8300(5) 0.2728(5) 0.5314(3) 0.1218(17) Uani 1 1 d . . .
O3 O 1.0442(4) 0.3049(5) 0.6082(3) 0.1189(17) Uani 1 1 d . . .
O4 O 0.8270(5) 0.3025(5) 0.6701(3) 0.1253(18) 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 0.0000 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'
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'
O O 0.0106 0.0060 '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
N2 Cr1 N6 176.51(18) . . ?
N2 Cr1 N1 82.62(18) . . ?
N6 Cr1 N1 100.30(16) . . ?
N2 Cr1 N5 95.62(17) . . ?
N6 Cr1 N5 82.28(17) . . ?
N1 Cr1 N5 94.70(15) . . ?
N2 Cr1 N4 79.39(19) . . ?
N6 Cr1 N4 97.91(17) . . ?
N1 Cr1 N4 160.98(18) . . ?
N5 Cr1 N4 93.13(15) . . ?
N2 Cr1 N8 103.23(17) . . ?
N6 Cr1 N8 78.84(18) . . ?
N1 Cr1 N8 88.93(16) . . ?
N5 Cr1 N8 161.12(18) . . ?
N4 Cr1 N8 89.24(15) . . ?
C7 N1 C1 118.3(4) . . ?
C7 N1 Cr1 113.7(3) . . ?
C1 N1 Cr1 127.3(3) . . ?
N3 N2 C12 120.0(4) . . ?
N3 N2 Cr1 122.7(3) . . ?
C12 N2 Cr1 117.1(3) . . ?
N2 N3 C13 108.5(4) . . ?
C17 N4 C13 118.8(5) . . ?
C17 N4 Cr1 129.4(4) . . ?
C13 N4 Cr1 111.8(4) . . ?
C6 C1 C2 119.8(5) . . ?
C6 C1 N1 120.2(5) . . ?
C2 C1 N1 120.0(5) . . ?
C1 C2 C3 119.9(6) . . ?
C4 C3 C2 120.5(7) . . ?
C5 C4 C3 119.6(7) . . ?
C4 C5 C6 121.2(7) . . ?
C1 C6 C5 119.0(6) . . ?
N1 C7 C8 127.0(5) . . ?
N1 C7 C12 116.2(5) . . ?
C8 C7 C12 116.7(5) . . ?
C9 C8 C7 119.7(5) . . ?
C8 C9 C10 122.5(6) . . ?
C11 C10 C9 120.5(6) . . ?
C10 C11 C12 117.8(5) . . ?
N2 C12 C11 127.6(5) . . ?
N2 C12 C7 109.7(5) . . ?
C11 C12 C7 122.7(5) . . ?
N4 C13 N3 117.6(5) . . ?
N4 C13 C14 121.8(6) . . ?
N3 C13 C14 120.7(6) . . ?
C15 C14 C13 117.1(6) . . ?
C14 C15 C16 122.1(6) . . ?
C17 C16 C15 117.8(6) . . ?
C16 C17 N4 122.4(6) . . ?
C24 N5 C18 120.9(4) . . ?
C24 N5 Cr1 113.5(3) . . ?
C18 N5 Cr1 125.4(3) . . ?
N7 N6 C29 119.7(4) . . ?
N7 N6 Cr1 122.8(3) . . ?
C29 N6 Cr1 117.5(3) . . ?
N6 N7 C30 108.7(4) . . ?
C34 N8 C30 119.0(4) . . ?
C34 N8 Cr1 129.0(4) . . ?
C30 N8 Cr1 112.0(3) . . ?
C19 C18 C23 118.9(5) . . ?
C19 C18 N5 120.6(5) . . ?
C23 C18 N5 120.3(4) . . ?
C18 C19 C20 120.3(5) . . ?
C21 C20 C19 120.3(5) . . ?
C20 C21 C22 119.8(5) . . ?
C21 C22 C23 120.0(5) . . ?
C22 C23 C18 120.6(5) . . ?
N5 C24 C29 116.2(4) . . ?
N5 C24 C25 126.3(5) . . ?
C29 C24 C25 117.4(5) . . ?
C26 C25 C24 118.1(5) . . ?
C25 C26 C27 123.7(5) . . ?
C28 C27 C26 119.0(5) . . ?
C27 C28 C29 119.1(5) . . ?
N6 C29 C28 127.0(5) . . ?
N6 C29 C24 110.4(4) . . ?
C28 C29 C24 122.5(5) . . ?
N8 C30 N7 117.7(4) . . ?
N8 C30 C31 121.7(5) . . ?
N7 C30 C31 120.6(5) . . ?
C32 C31 C30 118.4(6) . . ?
C31 C32 C33 120.2(5) . . ?
C32 C33 C34 119.2(6) . . ?
N8 C34 C33 121.5(5) . . ?
O1 Cl1 O3 110.8(3) . . ?
O1 Cl1 O4 110.4(3) . . ?
O3 Cl1 O4 106.7(3) . . ?
O1 Cl1 O2 110.8(3) . . ?
O3 Cl1 O2 108.2(3) . . ?
O4 Cl1 O2 109.9(3) . . ?
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 N2 1.861(4) . ?
Cr1 N6 1.871(4) . ?
Cr1 N1 1.906(4) . ?
Cr1 N5 1.920(4) . ?
Cr1 N4 1.947(4) . ?
Cr1 N8 1.959(4) . ?
N1 C7 1.346(6) . ?
N1 C1 1.436(6) . ?
N2 N3 1.308(5) . ?
N2 C12 1.384(6) . ?
N3 C13 1.386(6) . ?
N4 C17 1.364(6) . ?
N4 C13 1.369(6) . ?
C1 C6 1.376(6) . ?
C1 C2 1.381(6) . ?
C2 C3 1.381(7) . ?
C3 C4 1.364(8) . ?
C4 C5 1.359(8) . ?
C5 C6 1.392(7) . ?
C7 C8 1.412(6) . ?
C7 C12 1.424(6) . ?
C8 C9 1.356(7) . ?
C9 C10 1.397(7) . ?
C10 C11 1.364(7) . ?
C11 C12 1.401(6) . ?
C13 C14 1.392(7) . ?
C14 C15 1.380(7) . ?
C15 C16 1.387(8) . ?
C16 C17 1.363(7) . ?
N5 C24 1.365(5) . ?
N5 C18 1.429(5) . ?
N6 N7 1.303(5) . ?
N6 C29 1.387(5) . ?
N7 C30 1.384(6) . ?
N8 C34 1.345(5) . ?
N8 C30 1.359(6) . ?
C18 C19 1.372(6) . ?
C18 C23 1.379(6) . ?
C19 C20 1.380(7) . ?
C20 C21 1.368(7) . ?
C21 C22 1.366(6) . ?
C22 C23 1.378(6) . ?
C24 C29 1.405(6) . ?
C24 C25 1.415(6) . ?
C25 C26 1.373(6) . ?
C26 C27 1.391(7) . ?
C27 C28 1.357(6) . ?
C28 C29 1.398(6) . ?
C30 C31 1.388(6) . ?
C31 C32 1.370(7) . ?
C32 C33 1.377(7) . ?
C33 C34 1.378(6) . ?
Cl1 O1 1.412(4) . ?
Cl1 O3 1.420(4) . ?
Cl1 O4 1.424(4) . ?
Cl1 O2 1.429(4) . ?
