#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/27/1512790.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_1512790
loop_
_publ_author_name
'B. Shaabani'
'A.A. Khandar'
'M. Dusek'
'M. Pojarova'
'F. Mahmoudi'
_publ_section_title
;
 Synthesis, crystal structure, antimicrobial activity and electrochemistry
 study of chromium(III) and copper(II) complexes based on semicarbazone
 Schiff base and azide ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              563
_journal_page_last               568
_journal_paper_doi               10.1016/j.ica.2012.08.027
_journal_volume                  394
_journal_year                    2013
_chemical_formula_moiety         'C16 H20 Cr2 N14 O4'
_chemical_formula_sum            'C16 H20 Cr2 N14 O4'
_chemical_formula_weight         576.42
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 105.214(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7622(2)
_cell_length_b                   11.1757(2)
_cell_length_c                   11.8650(2)
_cell_measurement_reflns_used    7592
_cell_measurement_temperature    120
_cell_measurement_theta_max      67
_cell_measurement_theta_min      4
_cell_volume                     1121.14(4)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13892
_diffrn_reflns_theta_full        65.628
_diffrn_reflns_theta_max         66.967
_diffrn_reflns_theta_min         5.532
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.507
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.33
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.3138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         1976
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.0002503
_refine_ls_shift/su_mean         0.1301513
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 674. 900. 361. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0896
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0896
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                1724
_reflns_number_total             1986
_reflns_threshold_expression     I>2.0σ(I)
_cod_data_source_file            ICA-2013-394-563-568-1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               1512790
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,-y+1/2,z+1/2
-x+1/2,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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 1.1470(3) 0.2901(3) 0.5455(3) 0.0371 1.0000 Uani . . . .
O2 O 0.9113(3) 0.4429(2) 0.4191(3) 0.0340 1.0000 Uani . . . .
C1 C 0.7205(6) 0.5512(4) 0.6418(4) 0.0421 1.0000 Uani . . . .
C2 C 0.5747(6) 0.5644(5) 0.6669(5) 0.0493 1.0000 Uani . . . .
C3 C 0.4827(6) 0.4687(5) 0.6677(5) 0.0505 1.0000 Uani . . . .
C4 C 0.5322(5) 0.3573(5) 0.6425(4) 0.0451 1.0000 Uani . . . .
C5 C 0.6801(5) 0.3469(4) 0.6189(4) 0.0369 1.0000 Uani . . . .
C6 C 0.7426(5) 0.2353(4) 0.5911(4) 0.0406 1.0000 Uani . . . .
C7 C 1.1016(6) 0.1807(4) 0.5339(4) 0.0374 1.0000 Uani . . . .
C8 C 0.8598(6) 0.3593(4) 0.3260(4) 0.0441 1.0000 Uani . . . .
N1 N 0.7705(4) 0.4461(3) 0.6181(3) 0.0344 1.0000 Uani . . . .
N2 N 0.8819(4) 0.2397(3) 0.5720(3) 0.0362 1.0000 Uani . . . .
N3 N 0.9576(5) 0.1441(3) 0.5470(4) 0.0398 1.0000 Uani . . . .
N4 N 1.1889(4) 0.0967(4) 0.5044(3) 0.0426 1.0000 Uani . . . .
Cr1 Cr 0.98832(9) 0.39971(7) 0.58465(7) 0.0323 1.0000 Uani . . . .
N5 N 1.0834(4) 0.3780(4) 0.7561(4) 0.0395 1.0000 Uani . . . .
N6 N 1.0214(5) 0.3859(5) 0.8298(4) 0.0597 1.0000 Uani D . . .
N7 N 0.9711(13) 0.4292(12) 0.9084(11) 0.0782 0.5820 Uani D U 1 1
H2 H 1.1520 0.0191 0.5020 0.0500 1.0000 Uiso R . . .
H3 H 0.3906 0.4728 0.6883 0.0500 1.0000 Uiso R . . .
H4 H 1.2698 0.1159 0.4784 0.0500 1.0000 Uiso R . . .
H5 H 0.6925 0.1630 0.5970 0.0500 1.0000 Uiso R . . .
H12 H 0.4833 0.2879 0.6407 0.0500 1.0000 Uiso R . . .
H15 H 0.5456 0.6392 0.6750 0.0500 1.0000 Uiso R . . .
H18 H 0.7850 0.6143 0.6453 0.0500 1.0000 Uiso R . . .
H81 H 0.8281 0.4007 0.2537 0.0566 1.0000 Uiso R . . .
H82 H 0.9434 0.3058 0.3246 0.0566 1.0000 Uiso R . . .
H83 H 0.7726 0.3156 0.3383 0.0566 1.0000 Uiso R . . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cr -0.1635 2.4439 10.6406 6.1038 7.3537 0.3920 3.3240 20.2626 1.4922 98.7399
1.1832 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C7 . O1 Cr1 . 113.3(3) yes
Cr1 2_766 O2 C8 . 128.2(3) yes
Cr1 2_766 O2 Cr1 . 101.76(13) yes
C8 . O2 Cr1 . 124.8(3) yes
C2 . C1 N1 . 121.2(5) yes
C2 . C1 H18 . 120.5 no
N1 . C1 H18 . 118.2 no
C1 . C2 C3 . 120.3(5) yes
C1 . C2 H15 . 115.4 no
C3 . C2 H15 . 124.1 no
C2 . C3 C4 . 119.7(5) yes
C2 . C3 H3 . 122.9 no
C4 . C3 H3 . 117.4 no
C3 . C4 C5 . 118.6(5) yes
C3 . C4 H12 . 128.3 no
C5 . C4 H12 . 113.0 no
C4 . C5 C6 . 123.1(4) yes
C4 . C5 N1 . 120.2(4) yes
C6 . C5 N1 . 116.6(4) yes
C5 . C6 N2 . 116.1(4) yes
C5 . C6 H5 . 121.4 no
N2 . C6 H5 . 122.0 no
O1 . C7 N3 . 122.7(4) yes
O1 . C7 N4 . 121.6(4) yes
N3 . C7 N4 . 115.6(4) yes
O2 . C8 H81 . 109.9 no
O2 . C8 H82 . 109.7 no
H81 . C8 H82 . 109.5 no
O2 . C8 H83 . 108.8 no
H81 . C8 H83 . 109.5 no
H82 . C8 H83 . 109.5 no
C5 . N1 C1 . 120.0(4) yes
C5 . N1 Cr1 . 110.9(3) yes
C1 . N1 Cr1 . 129.0(3) yes
C6 . N2 N3 . 123.7(4) yes
C6 . N2 Cr1 . 117.4(3) yes
N3 . N2 Cr1 . 118.9(3) yes
C7 . N3 N2 . 108.2(3) yes
C7 . N4 H2 . 117.1 no
C7 . N4 H4 . 120.2 no
H2 . N4 H4 . 122.1 no
N1 . Cr1 Cr1 2_766 99.38(11) yes
N1 . Cr1 N2 . 78.92(15) yes
Cr1 2_766 Cr1 N2 . 135.76(12) yes
N1 . Cr1 O1 . 155.81(13) yes
Cr1 2_766 Cr1 O1 . 97.27(10) yes
N2 . Cr1 O1 . 76.91(14) yes
N1 . Cr1 O2 2_766 102.43(14) yes
Cr1 2_766 Cr1 O2 2_766 39.00(9) yes
N2 . Cr1 O2 2_766 174.60(16) yes
O1 . Cr1 O2 2_766 101.56(13) yes
N1 . Cr1 O2 . 92.13(14) yes
Cr1 2_766 Cr1 O2 . 39.24(8) yes
N2 . Cr1 O2 . 96.53(14) yes
O1 . Cr1 O2 . 89.74(13) yes
O2 2_766 Cr1 O2 . 78.24(13) yes
N1 . Cr1 N5 . 89.69(16) yes
Cr1 2_766 Cr1 N5 . 132.55(12) yes
N2 . Cr1 N5 . 91.67(16) yes
O1 . Cr1 N5 . 91.88(15) yes
O2 2_766 Cr1 N5 . 93.56(15) yes
O2 . Cr1 N5 . 171.79(15) yes
Cr1 . N5 N6 . 127.7(3) yes
N5 . N6 N7 . 160.6(10) yes
N5 . N6 N8 . 149.9(13) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C7 . 1.281(5) yes
O1 Cr1 . 1.997(3) yes
O2 Cr1 2_766 1.972(3) yes
O2 C8 . 1.426(5) yes
O2 Cr1 . 1.962(3) yes
C1 C2 . 1.394(6) yes
C1 N1 . 1.310(5) yes
C1 H18 . 0.897 no
C2 C3 . 1.342(7) yes
C2 H15 . 0.886 no
C3 C4 . 1.377(7) yes
C3 H3 . 0.904 no
C4 C5 . 1.401(6) yes
C4 H12 . 0.883 no
C5 C6 . 1.436(6) yes
C5 N1 . 1.364(5) yes
C6 N2 . 1.299(5) yes
C6 H5 . 0.931 no
C7 N3 . 1.374(6) yes
C7 N4 . 1.316(6) yes
C8 H81 . 0.950 no
C8 H82 . 0.950 no
C8 H83 . 0.950 no
N1 Cr1 . 2.114(4) yes
N2 N3 . 1.331(5) yes
N2 Cr1 . 2.004(4) yes
N4 H2 . 0.923 no
N4 H4 . 0.871 no
Cr1 Cr1 2_766 3.0525(16) yes
Cr1 N5 . 2.001(4) yes
N5 N6 . 1.147(6) yes
N6 N7 . 1.231(12) yes
N6 N8 . 1.154(18) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
N4 H2 N3 2_756 165 0.92 2.07 2.975(7) yes
N4 H4 N7 3_554 152 0.87 2.20 2.995(7) yes
N4 H4 N8 3_554 173 0.87 2.20 3.065(7) yes
C2 H15 N8 4_656 146 0.89 2.40 3.171(7) yes
