#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:58:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179164 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/25/4312504.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_4312504
loop_
_publ_author_name
'Torben Birk'
'Jesper Bendix'
_publ_contact_author
; 
Jesper Bendix
University of Copenhagen
Department of Chemistry 
Universitetsparken 5
DK-2100
Denmark 
;
_publ_contact_author_email       Bendix@kiku.dk
_publ_contact_author_fax         '45 35320133'
_publ_contact_author_phone       '45 35320101'
_publ_section_title
;
 Atom Transfer as a Preparative Tool in Coordination Chemistry. Synthesis
 and Characterization of Cr(V) Nitrido Complexes of Bidentate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7608
_journal_page_last               7615
_journal_paper_doi               10.1021/ic034777f
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C18 H12 Cr N3 O2'
_chemical_formula_sum            'C18 H12 Cr N3 O2'
_chemical_formula_weight         354.31
_chemical_name_common            Cr(N)(8-hydroxyquinoline)2
_chemical_name_systematic
; 
bis(8-hydroxyquinolinato)nitridochromium(V)
;
_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 and manual editing'
_cell_angle_alpha                80.519(6)
_cell_angle_beta                 75.721(7)
_cell_angle_gamma                75.131(5)
_cell_formula_units_Z            2
_cell_length_a                   7.2450(6)
_cell_length_b                   8.1710(4)
_cell_length_c                   13.1610(12)
_cell_measurement_reflns_used    102
_cell_measurement_temperature    122(1)
_cell_measurement_theta_max      22.9
_cell_measurement_theta_min      3.5
_cell_volume                     725.47(10)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg, 1998)'
_computing_molecular_graphics    'Ortep (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'θ and φ 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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            69245
_diffrn_reflns_theta_full        40.00
_diffrn_reflns_theta_max         40.00
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gausian Integration (---, 1970)
;
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             362
_exptl_crystal_size_max          0.351
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.120
_refine_diff_density_max         .606
_refine_diff_density_min         -.601
_refine_diff_density_rms         .068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         8981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0332P)²+0.2543P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0745
_reflns_number_gt                8264
_reflns_number_total             8981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034777fsi20030707_095115_1.cif
_cod_data_source_block           qui
_cod_database_code               4312504
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 0.661515(15) 0.794547(13) 0.235462(8) 0.01085(2) Uani 1 1 d . . .
O1 O 0.50132(8) 0.94736(6) 0.33676(4) 0.01301(8) Uani 1 1 d . . .
O2 O 0.67252(9) 0.69361(6) 0.11080(4) 0.01501(8) Uani 1 1 d . . .
N1 N 0.48649(8) 0.63862(7) 0.32114(4) 0.01175(8) Uani 1 1 d . . .
N2 N 0.72076(8) 0.99334(7) 0.12668(4) 0.01088(8) Uani 1 1 d . . .
C8 C 0.38474(9) 0.87589(8) 0.41658(5) 0.01073(8) Uani 1 1 d . . .
C18 C 0.73680(9) 0.95632(8) 0.02707(5) 0.01045(8) Uani 1 1 d . . .
C9 C 0.37209(9) 0.70738(7) 0.40952(5) 0.01028(8) Uani 1 1 d . . .
C10 C 0.74183(10) 1.14379(8) 0.14042(5) 0.01283(9) Uani 1 1 d . . .
H10 H 0.7337 1.1620 0.2092 0.015 Uiso 1 1 d R . .
C4 C 0.25231(9) 0.61745(8) 0.48788(5) 0.01155(8) Uani 1 1 d . . .
C13 C 0.77559(9) 1.07287(8) -0.06300(5) 0.01144(8) Uani 1 1 d . . .
C7 C 0.27391(10) 0.95217(8) 0.50514(5) 0.01301(9) Uani 1 1 d . . .
H7 H 0.2820 1.0606 0.5126 0.016 Uiso 1 1 d R . .
C14 C 0.78963(10) 1.02192(9) -0.16286(5) 0.01415(10) Uani 1 1 d . . .
H14 H 0.8194 1.0869 -0.2185 0.017 Uiso 1 1 d R . .
C16 C 0.72658(10) 0.74600(9) -0.07815(5) 0.01398(9) Uani 1 1 d . . .
H16 H 0.7173 0.6347 -0.0856 0.017 Uiso 1 1 d R . .
C11 C 0.77980(10) 1.26810(8) 0.05533(5) 0.01418(10) Uani 1 1 d . . .
H11 H 0.7894 1.3749 0.0698 0.017 Uiso 1 1 d R . .
C5 C 0.14193(10) 0.69965(9) 0.57777(5) 0.01401(9) Uani 1 1 d . . .
H5 H 0.0613 0.6352 0.6285 0.017 Uiso 1 1 d R . .
C2 C 0.36756(11) 0.38494(8) 0.37914(5) 0.01493(10) Uani 1 1 d . . .
H2 H 0.3724 0.2780 0.3643 0.018 Uiso 1 1 d R . .
C1 C 0.48258(11) 0.48364(8) 0.30566(5) 0.01442(10) Uani 1 1 d . . .
H1 H 0.5728 0.4434 0.2437 0.017 Uiso 1 1 d R . .
C12 C 0.79691(10) 1.23254(8) -0.04571(5) 0.01378(9) Uani 1 1 d . . .
H12 H 0.8280 1.3092 -0.1005 0.017 Uiso 1 1 d R . .
C17 C 0.71115(9) 0.79134(8) 0.02085(5) 0.01146(8) Uani 1 1 d . . .
C15 C 0.76563(10) 0.86224(9) -0.16862(5) 0.01489(10) Uani 1 1 d . . .
H15 H 0.7689 0.8341 -0.2333 0.018 Uiso 1 1 d R . .
C6 C 0.15441(10) 0.86283(9) 0.58422(5) 0.01431(10) Uani 1 1 d . . .
H6 H 0.0823 0.9146 0.6398 0.017 Uiso 1 1 d R . .
C3 C 0.25458(10) 0.45067(8) 0.47014(5) 0.01370(9) Uani 1 1 d . . .
H3 H 0.1765 0.3820 0.5209 0.016 Uiso 1 1 d R . .
N3 N 0.85805(10) 0.71799(9) 0.27127(5) 0.01813(10) 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
Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .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
N3 Cr1 O1 106.85(3) . . y
N3 Cr1 O2 107.85(3) . . y
O1 Cr1 O2 145.25(3) . . ?
N3 Cr1 N1 102.86(3) . . y
O1 Cr1 N1 81.67(2) . . ?
O2 Cr1 N1 89.01(2) . . y
N3 Cr1 N2 103.39(3) . . y
O1 Cr1 N2 91.63(2) . . y
O2 Cr1 N2 82.12(2) . . ?
N1 Cr1 N2 153.73(2) . . ?
C8 O1 Cr1 114.48(4) . . ?
C17 O2 Cr1 114.76(4) . . ?
C1 N1 C9 119.49(5) . . ?
C1 N1 Cr1 129.18(5) . . ?
C9 N1 Cr1 111.13(4) . . ?
C10 N2 C18 119.37(5) . . ?
C10 N2 Cr1 129.76(4) . . ?
C18 N2 Cr1 110.87(4) . . ?
O1 C8 C7 125.50(6) . . ?
O1 C8 C9 117.09(5) . . ?
C7 C8 C9 117.41(5) . . ?
N2 C18 C13 122.47(6) . . ?
N2 C18 C17 114.97(5) . . ?
C13 C18 C17 122.56(5) . . ?
N1 C9 C4 122.45(5) . . ?
N1 C9 C8 114.57(5) . . ?
C4 C9 C8 122.98(5) . . ?
N2 C10 C11 122.08(6) . . ?
N2 C10 H10 116.3 . . ?
C11 C10 H10 121.6 . . ?
C9 C4 C3 116.70(6) . . ?
C9 C4 C5 117.88(6) . . ?
C3 C4 C5 125.41(6) . . ?
C18 C13 C12 116.81(6) . . ?
C18 C13 C14 118.04(6) . . ?
C12 C13 C14 125.15(6) . . ?
C8 C7 C6 120.00(6) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 H7 120.8 . . ?
C15 C14 C13 119.25(6) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.1 . . ?
C17 C16 C15 119.95(6) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C12 C11 C10 119.26(6) . . ?
C12 C11 H11 122.1 . . ?
C10 C11 H11 118.6 . . ?
C6 C5 C4 118.94(6) . . ?
C6 C5 H5 125.7 . . ?
C4 C5 H5 115.3 . . ?
C3 C2 C1 119.33(6) . . ?
C3 C2 H2 122.8 . . ?
C1 C2 H2 117.9 . . ?
N1 C1 C2 122.01(6) . . ?
N1 C1 H1 113.6 . . ?
C2 C1 H1 124.1 . . ?
C11 C12 C13 120.01(6) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 120.4 . . ?
O2 C17 C16 125.03(6) . . ?
O2 C17 C18 117.28(5) . . ?
C16 C17 C18 117.70(6) . . ?
C14 C15 C16 122.50(6) . . ?
C14 C15 H15 117.8 . . ?
C16 C15 H15 119.6 . . ?
C5 C6 C7 122.77(6) . . ?
C5 C6 H6 118.4 . . ?
C7 C6 H6 118.8 . . ?
C2 C3 C4 119.99(6) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 120.9 . . ?
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 N3 1.5549(7) . y
Cr1 O1 1.9300(5) . y
Cr1 O2 1.9303(5) . y
Cr1 N1 2.0380(6) . y
Cr1 N2 2.0399(6) . y
O1 C8 1.3309(8) . ?
O2 C17 1.3256(8) . ?
N1 C1 1.3237(8) . ?
N1 C9 1.3625(8) . ?
N2 C10 1.3230(8) . ?
N2 C18 1.3642(8) . ?
C8 C7 1.3829(9) . ?
C8 C9 1.4226(8) . ?
C18 C13 1.4114(8) . ?
C18 C17 1.4251(9) . ?
C9 C4 1.4117(9) . ?
C10 C11 1.4065(9) . ?
C10 H10 0.9260 . ?
C4 C3 1.4153(9) . ?
C4 C5 1.4176(9) . ?
C13 C12 1.4129(9) . ?
C13 C14 1.4154(9) . ?
C7 C6 1.4126(9) . ?
C7 H7 0.9247 . ?
C14 C15 1.3762(10) . ?
C14 H14 0.8465 . ?
C16 C17 1.3833(9) . ?
C16 C15 1.4138(10) . ?
C16 H16 0.9513 . ?
C11 C12 1.3768(10) . ?
C11 H11 0.9458 . ?
C5 C6 1.3770(10) . ?
C5 H5 0.9558 . ?
C2 C3 1.3769(10) . ?
C2 C1 1.4037(10) . ?
C2 H2 0.9166 . ?
C1 H1 0.9568 . ?
C12 H12 0.8980 . ?
C15 H15 0.9108 . ?
C6 H6 0.8874 . ?
C3 H3 0.9664 . ?
