#------------------------------------------------------------------------------
#$Date: 2016-01-24 04:15:28 +0200 (Sun, 24 Jan 2016) $
#$Revision: 174896 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500012.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_1500012
loop_
_publ_author_name
'Raj Pal Sharma'
'Rajni Sharma'
'Ritu Bala'
'Juan M. Salas'
'Miguel Quirós'
_publ_contact_author_address
;
     Departamento de Química Inorgánica
     Facultad de Ciencias
     Universidad de Granada
     18071 Granada
     SPAIN
;
_publ_contact_author_email       mquiros@ugr.es
_publ_contact_author_fax         34-58-248526
_publ_contact_author_name        'Miguel Quirós'
_publ_contact_author_phone       34-58-240441
_publ_section_title
;
 Synthesis, spectroscopic characterisation and
 X-ray structure of [trans-Co(en)₂(NO₂)₂]₂(Cr₂O₇)
;
_journal_issue                   10
_journal_name_full               'Journal of Chemical Crystallography'
_journal_page_first              769
_journal_page_last               775
_journal_paper_doi               10.1007/s10870-005-3886-9
_journal_volume                  35
_journal_year                    2005
_chemical_formula_sum            'C8 H32 Co2 Cr2 N12 O15'
_chemical_formula_weight         758.32
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.778(2)
_cell_length_b                   30.457(2)
_cell_length_c                   6.5364(5)
_cell_measurement_reflns_used    2692
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.68
_cell_volume                     4932.8(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Xtal_GX (S. Hall & D. du Boulay)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7639
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_number         182
_exptl_absorpt_coefficient_mu    2.273
_exptl_absorpt_correction_T_max  0.8391
_exptl_absorpt_correction_T_min  0.6620
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2779
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0800P)²+50.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                2556
_reflns_number_total             2779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            conitdcr.cif
_cod_data_source_block           conitdcr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthorrombic' was replaced with
'orthorhombic' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               1500012
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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
Co Co 0.44299(3) 0.36255(3) 0.37586(13) 0.0228(2) Uani 1 1 d .
N1N N 0.4014(2) 0.3803(2) 0.6120(10) 0.0411(15) Uani 1 1 d .
O1N O 0.4223(2) 0.3816(2) 0.7777(10) 0.0570(16) Uani 1 1 d .
O2N O 0.3558(3) 0.3908(5) 0.5990(10) 0.137(5) Uani 1 1 d .
N2N N 0.4828(2) 0.3423(2) 0.1365(10) 0.0364(13) Uani 1 1 d .
O3N O 0.5169(2) 0.3649(3) 0.0559(11) 0.0654(19) Uani 1 1 d .
O4N O 0.4719(4) 0.3063(2) 0.0600(10) 0.077(2) Uani 1 1 d .
N1 N 0.5027(2) 0.34451(18) 0.5515(9) 0.0274(11) Uani 1 1 d .
H11 H 0.5341 0.3546 0.5007 0.033 Uiso 1 1 d R
H12 H 0.4982 0.3558 0.6777 0.033 Uiso 1 1 d R
C1 C 0.5040(3) 0.2960(2) 0.5623(11) 0.0334(14) Uani 1 1 d .
H13 H 0.5245 0.2865 0.6808 0.040 Uiso 1 1 d R
H14 H 0.5210 0.2841 0.4407 0.040 Uiso 1 1 d R
C2 C 0.4477(3) 0.2801(3) 0.5769(12) 0.0377(16) Uani 1 1 d .
H21 H 0.4463 0.2487 0.5536 0.045 Uiso 1 1 d R
H22 H 0.4333 0.2861 0.7120 0.045 Uiso 1 1 d R
N2 N 0.4154(2) 0.3036(2) 0.4184(9) 0.0383(14) Uani 1 1 d .
H23 H 0.3807 0.3050 0.4580 0.046 Uiso 1 1 d R
H24 H 0.4168 0.2886 0.2999 0.046 Uiso 1 1 d R
N3 N 0.3842(2) 0.3810(2) 0.1951(8) 0.0303(12) Uani 1 1 d .
H31 H 0.3877 0.3680 0.0721 0.036 Uiso 1 1 d R
H32 H 0.3523 0.3729 0.2490 0.036 Uiso 1 1 d R
C3 C 0.4417(4) 0.4436(3) 0.1712(19) 0.060(3) Uani 1 1 d .
H33 H 0.4433 0.4752 0.1891 0.072 Uiso 1 1 d R
H34 H 0.4584 0.4363 0.0414 0.072 Uiso 1 1 d R
C4 C 0.3859(3) 0.4290(3) 0.1724(14) 0.047(2) Uani 1 1 d .
H41 H 0.3686 0.4375 0.0452 0.056 Uiso 1 1 d R
H42 H 0.3666 0.4429 0.2843 0.056 Uiso 1 1 d R
N4 N 0.4708(2) 0.4213(2) 0.3417(11) 0.0416(15) Uani 1 1 d .
H43 H 0.4664 0.4366 0.4584 0.050 Uiso 1 1 d R
H44 H 0.5063 0.4202 0.3134 0.050 Uiso 1 1 d R
Cr Cr 0.56056(6) 0.47649(5) 0.6988(2) 0.0570(5) Uani 1 1 d D
O1D O 0.4845(5) 0.4789(4) 0.679(2) 0.058(3) Uiso 0.50 1 d P
O2D O 0.5750(4) 0.4367(3) 0.5491(15) 0.045(2) Uiso 0.50 1 d PD
O3D O 0.5655(4) 0.4571(3) 0.9359(11) 0.041(2) Uiso 0.50 1 d PD
O4D O 0.5915(6) 0.5204(3) 0.674(2) 0.084(5) Uiso 0.50 1 d PD
O2D' O 0.5752(6) 0.4697(5) 0.4491(13) 0.076(4) Uiso 0.50 1 d PD
O3D' O 0.5430(9) 0.4306(5) 0.786(3) 0.126(8) Uiso 0.50 1 d PD
O4D' O 0.6170(4) 0.4956(4) 0.792(2) 0.069(4) Uiso 0.50 1 d PD
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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
N4 Co N1N 91.4(3) . .
N4 Co N2 178.4(3) . .
N1N Co N2 87.5(3) . .
N4 Co N2N 91.1(3) . .
N1N Co N2N 177.4(3) . .
N2 Co N2N 90.1(3) . .
N4 Co N1 93.4(2) . .
N1N Co N1 90.8(2) . .
N2 Co N1 85.5(2) . .
N2N Co N1 90.0(2) . .
N4 Co N3 86.0(2) . .
N1N Co N3 90.3(2) . .
N2 Co N3 95.1(2) . .
N2N Co N3 89.0(2) . .
N1 Co N3 178.8(2) . .
O2N N1N O1N 118.1(7) . .
O2N N1N Co 122.0(6) . .
O1N N1N Co 119.9(5) . .
O3N N2N O4N 118.8(7) . .
O3N N2N Co 121.5(6) . .
O4N N2N Co 119.6(6) . .
C1 N1 Co 109.0(4) . .
C2 C1 N1 108.0(6) . .
C1 C2 N2 107.7(6) . .
C2 N2 Co 110.7(4) . .
C4 N3 Co 109.0(4) . .
C4 C3 N4 108.6(8) . .
C3 C4 N3 109.3(6) . .
C3 N4 Co 109.6(5) . .
O4D Cr O2D 118.6(7) . .
O3D' Cr O4D' 114.8(8) . .
O4D Cr O3D 111.5(6) . .
O2D Cr O3D 106.6(5) . .
O3D' Cr O2D' 107.6(8) . .
O4D' Cr O2D' 102.7(6) . .
O3D' Cr O1D 122.4(10) . 2_665
O4D' Cr O1D 107.2(7) . 2_665
O2D' Cr O1D 99.2(7) . 2_665
O4D Cr O1D 116.9(7) . .
O2D Cr O1D 102.2(6) . .
O3D Cr O1D 98.7(6) . .
Cr O1D Cr 131.0(7) 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co N4 1.930(6) .
Co N1N 1.933(6) .
Co N2 1.940(6) .
Co N2N 1.949(6) .
Co N1 1.952(5) .
Co N3 1.958(6) .
N1N O2N 1.175(8) .
N1N O1N 1.202(9) .
N2N O3N 1.210(9) .
N2N O4N 1.237(9) .
N1 C1 1.481(9) .
C1 C2 1.478(10) .
C2 N2 1.493(9) .
N3 C4 1.472(10) .
C3 C4 1.451(11) .
C3 N4 1.491(11) .
Cr O4D 1.549(8) .
Cr O3D' 1.571(9) .
Cr O2D 1.597(7) .
Cr O4D' 1.633(8) .
Cr O3D 1.663(7) .
Cr O2D' 1.684(8) .
Cr O1D 1.765(13) 2_665
Cr O1D 1.889(13) .
