#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:55:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179353 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/50/4325043.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_4325043
loop_
_publ_author_name
'Alexis D. Ostrowski'
'Ryan O. Absalonson'
'Malcolm A. De Leo'
'Guang Wu'
'James G. Pavlovich'
'Janet Adamson'
'Bilal Azhar'
'Alexei V. Iretskii'
'Ian L. Megson'
'Peter C. Ford'
_publ_section_title
;
 Photochemistry of trans-Cr(cyclam)(ONO)2+, a Nitric Oxide Precursor
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4453
_journal_page_last               4462
_journal_paper_doi               10.1021/ic200094x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C10 H26 Cl Cr N4 O7'
_chemical_formula_weight         401.80
_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                98.812(5)
_cell_angle_beta                 106.707(5)
_cell_angle_gamma                114.349(4)
_cell_formula_units_Z            2
_cell_length_a                   9.518(3)
_cell_length_b                   9.950(3)
_cell_length_c                   10.948(4)
_cell_measurement_temperature    293(2)
_cell_volume                     859.7(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega scan'
_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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6876
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  0.614
_exptl_absorpt_correction_T_min  0.506
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.121(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3341
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1052P)²+2.2433P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1949
_refine_ls_wR_factor_ref         0.2010
_reflns_number_gt                2917
_reflns_number_total             3341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200094x_si_002.cif
_cod_data_source_block           f112509
_cod_database_code               4325043
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
C1 C 0.1488(6) 0.3240(6) 0.9388(5) 0.0476(12) Uani 1 1 d .
H1A H 0.0336 0.2890 0.8814 0.057 Uiso 1 1 calc R
H1B H 0.1571 0.3367 1.0307 0.057 Uiso 1 1 calc R
C2 C 0.2018(6) 0.2052(5) 0.8966(5) 0.0450(11) Uani 1 1 d .
H2A H 0.1350 0.1079 0.9089 0.054 Uiso 1 1 calc R
H2B H 0.1848 0.1861 0.8026 0.054 Uiso 1 1 calc R
C3 C 0.4550(7) 0.1752(5) 0.9321(5) 0.0484(12) Uani 1 1 d .
H3A H 0.4423 0.1725 0.8404 0.058 Uiso 1 1 calc R
H3B H 0.3944 0.0694 0.9321 0.058 Uiso 1 1 calc R
C4 C 0.6401(7) 0.2429(6) 1.0193(5) 0.0500(12) Uani 1 1 d .
H4A H 0.6530 0.2582 1.1123 0.060 Uiso 1 1 calc R
H4B H 0.6755 0.1674 0.9960 0.060 Uiso 1 1 calc R
C5 C 0.2440(6) 0.6046(6) 0.9928(5) 0.0458(11) Uani 1 1 d .
H5A H 0.2695 0.6131 1.0869 0.055 Uiso 1 1 calc R
H5B H 0.1291 0.5834 0.9520 0.055 Uiso 1 1 calc R
C6 C 0.8779(8) 0.1767(6) 0.3815(6) 0.0620(16) Uani 1 1 d .
H6A H 0.7998 0.1637 0.2953 0.074 Uiso 1 1 calc R
H6B H 0.8980 0.0884 0.3727 0.074 Uiso 1 1 calc R
C7 C 0.8055(7) 0.1837(6) 0.4839(7) 0.0606(15) Uani 1 1 d .
H7A H 0.8790 0.1881 0.5686 0.073 Uiso 1 1 calc R
H7B H 0.6976 0.0919 0.4554 0.073 Uiso 1 1 calc R
C8 C 0.7424(8) 0.3618(8) 0.6169(6) 0.0647(17) Uani 1 1 d .
H8A H 0.8281 0.3732 0.6979 0.078 Uiso 1 1 calc R
H8B H 0.6371 0.2756 0.6051 0.078 Uiso 1 1 calc R
C9 C 0.7277(9) 0.5083(10) 0.6329(7) 0.0699(19) Uani 1 1 d .
H9A H 0.6737 0.5125 0.6952 0.084 Uiso 1 1 calc R
H9B H 0.6554 0.5024 0.5469 0.084 Uiso 1 1 calc R
C10 C 1.1077(8) 0.3423(8) 0.3172(6) 0.0627(16) Uani 1 1 d .
H10A H 1.0277 0.3431 0.2393 0.075 Uiso 1 1 calc R
H10B H 1.1251 0.2548 0.2899 0.075 Uiso 1 1 calc R
Cl Cl 0.32631(17) 0.06708(16) 0.25270(14) 0.0543(4) Uani 1 1 d .
Cr1 Cr 0.5000 0.5000 1.0000 0.0260(3) Uani 1 2 d S
Cr2 Cr 1.0000 0.5000 0.5000 0.0277(3) Uani 1 2 d S
H31 H 0.702(8) 0.759(9) 0.473(4) 0.12(3) Uiso 1 1 d D
H32 H 0.652(4) 0.690(5) 0.335(3) 0.051(15) Uiso 1 1 d D
N1 N 0.2614(4) 0.4747(4) 0.9271(4) 0.0348(8) Uani 1 1 d .
H1 H 0.232(7) 0.466(6) 0.838(6) 0.042 Uiso 1 1 calc .
N2 N 0.3815(5) 0.2674(4) 0.9806(4) 0.0369(8) Uani 1 1 d .
H2 H 0.388(7) 0.261(6) 1.064(6) 0.044 Uiso 1 1 calc .
N3 N 1.0387(5) 0.3231(5) 0.4225(4) 0.0434(9) Uani 1 1 d .
H3 H 1.115(8) 0.319(7) 0.492(6) 0.052 Uiso 1 1 calc .
N4 N 0.7856(5) 0.3265(5) 0.5002(4) 0.0444(9) Uani 1 1 d .
H4 H 0.699(8) 0.308(7) 0.425(6) 0.053 Uiso 1 1 calc .
O1 O 0.5071(3) 0.5466(3) 1.1758(2) 0.0258(6) Uani 1 1 d .
O2 O 0.8795(3) 0.4902(3) 0.3263(2) 0.0274(6) Uani 1 1 d .
O3 O 0.7396(5) 0.7676(5) 0.4066(4) 0.0603(10) Uani 1 1 d D
O4 O 0.295(2) 0.0975(18) 0.3585(11) 0.254(8) Uani 1 1 d .
O5 O 0.4599(10) 0.1805(15) 0.2504(10) 0.279(10) Uani 1 1 d .
O6 O 0.350(2) -0.0547(15) 0.2575(10) 0.237(8) Uani 1 1 d .
O7 O 0.2006(8) 0.0364(12) 0.1320(8) 0.156(4) 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'
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'
Cl Cl 0.1484 0.1585 '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
N1 C1 C2 108.4(4) . .
N1 C1 H1A 110.0 . .
C2 C1 H1A 110.0 . .
N1 C1 H1B 110.0 . .
C2 C1 H1B 110.0 . .
H1A C1 H1B 108.4 . .
N2 C2 C1 108.4(4) . .
N2 C2 H2A 110.0 . .
C1 C2 H2A 110.0 . .
N2 C2 H2B 110.0 . .
C1 C2 H2B 110.0 . .
H2A C2 H2B 108.4 . .
N2 C3 C4 111.9(4) . .
N2 C3 H3A 109.2 . .
C4 C3 H3A 109.2 . .
N2 C3 H3B 109.2 . .
C4 C3 H3B 109.2 . .
H3A C3 H3B 107.9 . .
C5 C4 C3 115.2(4) 2_667 .
C5 C4 H4A 108.5 2_667 .
C3 C4 H4A 108.5 . .
C5 C4 H4B 108.5 2_667 .
C3 C4 H4B 108.5 . .
H4A C4 H4B 107.5 . .
N1 C5 C4 111.7(4) . 2_667
N1 C5 H5A 109.3 . .
C4 C5 H5A 109.3 2_667 .
N1 C5 H5B 109.3 . .
C4 C5 H5B 109.3 2_667 .
H5A C5 H5B 108.0 . .
C7 C6 N3 109.6(4) . .
C7 C6 H6A 109.8 . .
N3 C6 H6A 109.8 . .
C7 C6 H6B 109.8 . .
N3 C6 H6B 109.8 . .
H6A C6 H6B 108.2 . .
C6 C7 N4 108.0(4) . .
C6 C7 H7A 110.1 . .
N4 C7 H7A 110.1 . .
C6 C7 H7B 110.1 . .
N4 C7 H7B 110.1 . .
H7A C7 H7B 108.4 . .
N4 C8 C9 112.0(4) . .
N4 C8 H8A 109.2 . .
C9 C8 H8A 109.2 . .
N4 C8 H8B 109.2 . .
C9 C8 H8B 109.2 . .
H8A C8 H8B 107.9 . .
C8 C9 C10 115.0(5) . 2_766
C8 C9 H9A 108.5 . .
C10 C9 H9A 108.5 2_766 .
C8 C9 H9B 108.5 . .
C10 C9 H9B 108.5 2_766 .
H9A C9 H9B 107.5 . .
N3 C10 C9 111.4(5) . 2_766
N3 C10 H10A 109.4 . .
C9 C10 H10A 109.4 2_766 .
N3 C10 H10B 109.4 . .
C9 C10 H10B 109.4 2_766 .
H10A C10 H10B 108.0 . .
O4 Cl O5 114.6(11) . .
O4 Cl O6 103.8(6) . .
O5 Cl O6 109.4(11) . .
O4 Cl O7 114.5(8) . .
O5 Cl O7 103.1(4) . .
O6 Cl O7 111.5(8) . .
O1 Cr1 O1 180.000(1) 2_667 .
O1 Cr1 N2 90.70(14) 2_667 .
O1 Cr1 N2 89.30(14) . .
O1 Cr1 N2 89.30(14) 2_667 2_667
O1 Cr1 N2 90.70(14) . 2_667
N2 Cr1 N2 180.000(1) . 2_667
O1 Cr1 N1 89.44(13) 2_667 2_667
O1 Cr1 N1 90.56(13) . 2_667
N2 Cr1 N1 94.60(15) . 2_667
N2 Cr1 N1 85.40(15) 2_667 2_667
O1 Cr1 N1 90.56(13) 2_667 .
O1 Cr1 N1 89.44(13) . .
N2 Cr1 N1 85.40(15) . .
N2 Cr1 N1 94.60(15) 2_667 .
N1 Cr1 N1 180.000(1) 2_667 .
O2 Cr2 O2 180.0 2_766 .
O2 Cr2 N3 89.13(14) 2_766 .
O2 Cr2 N3 90.87(14) . .
O2 Cr2 N3 90.87(14) 2_766 2_766
O2 Cr2 N3 89.13(14) . 2_766
N3 Cr2 N3 180.000(2) . 2_766
O2 Cr2 N4 90.16(15) 2_766 2_766
O2 Cr2 N4 89.84(14) . 2_766
N3 Cr2 N4 94.68(18) . 2_766
N3 Cr2 N4 85.32(18) 2_766 2_766
O2 Cr2 N4 89.84(14) 2_766 .
O2 Cr2 N4 90.16(15) . .
N3 Cr2 N4 85.32(18) . .
N3 Cr2 N4 94.68(18) 2_766 .
N4 Cr2 N4 180.0(2) 2_766 .
C5 N1 C1 112.2(4) . .
C5 N1 Cr1 114.9(3) . .
C1 N1 Cr1 106.1(3) . .
C5 N1 H1 108(3) . .
C1 N1 H1 108(3) . .
Cr1 N1 H1 108(3) . .
C2 N2 C3 113.1(4) . .
C2 N2 Cr1 106.9(3) . .
C3 N2 Cr1 116.0(3) . .
C2 N2 H2 107(4) . .
C3 N2 H2 107(3) . .
Cr1 N2 H2 107(3) . .
C10 N3 C6 114.5(5) . .
C10 N3 Cr2 115.9(3) . .
C6 N3 Cr2 106.2(3) . .
C10 N3 H3 106(4) . .
C6 N3 H3 107(4) . .
Cr2 N3 H3 106(4) . .
C8 N4 C7 113.2(4) . .
C8 N4 Cr2 115.6(4) . .
C7 N4 Cr2 106.1(3) . .
C8 N4 H4 107(4) . .
C7 N4 H4 107(4) . .
Cr2 N4 H4 107(4) . .
H31 O3 H32 102.7(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.491(6) .
C1 C2 1.525(8) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 N2 1.484(6) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 N2 1.485(7) .
C3 C4 1.526(8) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C5 1.517(8) 2_667
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 N1 1.474(6) .
C5 C4 1.517(8) 2_667
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 C7 1.481(10) .
C6 N3 1.494(7) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 N4 1.500(7) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 N4 1.486(7) .
C8 C9 1.509(10) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C10 1.517(10) 2_766
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 N3 1.482(7) .
C10 C9 1.517(10) 2_766
C10 H10A 0.9700 .
C10 H10B 0.9700 .
Cl O4 1.302(7) .
Cl O5 1.317(7) .
Cl O6 1.327(7) .
Cl O7 1.392(6) .
Cr1 O1 1.884(2) 2_667
Cr1 O1 1.884(2) .
Cr1 N2 2.057(4) .
Cr1 N2 2.057(4) 2_667
Cr1 N1 2.070(4) 2_667
Cr1 N1 2.070(4) .
Cr2 O2 1.881(2) 2_766
Cr2 O2 1.881(2) .
Cr2 N3 2.052(4) .
Cr2 N3 2.052(4) 2_766
Cr2 N4 2.060(4) 2_766
Cr2 N4 2.060(4) .
N1 H1 0.91(6) .
N2 H2 0.90(6) .
N3 H3 0.91(6) .
N4 H4 0.91(7) .
O3 H31 0.896(10) .
O3 H32 0.898(10) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 C1 C2 N2 56.0(5) . .
N2 C3 C4 C5 -70.5(6) . 2_667
N3 C6 C7 N4 56.2(6) . .
N4 C8 C9 C10 -72.0(7) . 2_766
C4 C5 N1 C1 179.7(4) 2_667 .
C4 C5 N1 Cr1 58.4(4) 2_667 .
C2 C1 N1 C5 -167.7(4) . .
C2 C1 N1 Cr1 -41.4(4) . .
O1 Cr1 N1 C5 -129.4(3) 2_667 .
O1 Cr1 N1 C5 50.6(3) . .
N2 Cr1 N1 C5 139.9(3) . .
N2 Cr1 N1 C5 -40.1(3) 2_667 .
N1 Cr1 N1 C5 11(100) 2_667 .
O1 Cr1 N1 C1 105.9(3) 2_667 .
O1 Cr1 N1 C1 -74.1(3) . .
N2 Cr1 N1 C1 15.3(3) . .
N2 Cr1 N1 C1 -164.7(3) 2_667 .
N1 Cr1 N1 C1 -114(100) 2_667 .
C1 C2 N2 C3 -169.4(4) . .
C1 C2 N2 Cr1 -40.5(4) . .
C4 C3 N2 C2 179.3(4) . .
C4 C3 N2 Cr1 55.3(5) . .
O1 Cr1 N2 C2 -76.5(3) 2_667 .
O1 Cr1 N2 C2 103.5(3) . .
N2 Cr1 N2 C2 63(100) 2_667 .
N1 Cr1 N2 C2 -166.0(3) 2_667 .
N1 Cr1 N2 C2 14.0(3) . .
O1 Cr1 N2 C3 50.7(3) 2_667 .
O1 Cr1 N2 C3 -129.3(3) . .
N2 Cr1 N2 C3 -170(100) 2_667 .
N1 Cr1 N2 C3 -38.8(3) 2_667 .
N1 Cr1 N2 C3 141.2(3) . .
C9 C10 N3 C6 -178.9(5) 2_766 .
C9 C10 N3 Cr2 56.9(5) 2_766 .
C7 C6 N3 C10 -169.6(4) . .
C7 C6 N3 Cr2 -40.4(5) . .
O2 Cr2 N3 C10 -128.8(4) 2_766 .
O2 Cr2 N3 C10 51.2(4) . .
N3 Cr2 N3 C10 119(100) 2_766 .
N4 Cr2 N3 C10 -38.8(4) 2_766 .
N4 Cr2 N3 C10 141.2(4) . .
O2 Cr2 N3 C6 102.8(3) 2_766 .
O2 Cr2 N3 C6 -77.2(3) . .
N3 Cr2 N3 C6 -10(100) 2_766 .
N4 Cr2 N3 C6 -167.2(3) 2_766 .
N4 Cr2 N3 C6 12.8(3) . .
C9 C8 N4 C7 178.5(5) . .
C9 C8 N4 Cr2 55.9(6) . .
C6 C7 N4 C8 -169.8(5) . .
C6 C7 N4 Cr2 -42.0(5) . .
O2 Cr2 N4 C8 52.9(4) 2_766 .
O2 Cr2 N4 C8 -127.1(4) . .
N3 Cr2 N4 C8 142.0(4) . .
N3 Cr2 N4 C8 -38.0(4) 2_766 .
N4 Cr2 N4 C8 -168(100) 2_766 .
O2 Cr2 N4 C7 -73.4(3) 2_766 .
O2 Cr2 N4 C7 106.6(3) . .
N3 Cr2 N4 C7 15.7(3) . .
N3 Cr2 N4 C7 -164.3(3) 2_766 .
N4 Cr2 N4 C7 66(100) 2_766 .
