#------------------------------------------------------------------------------
#$Date: 2017-05-04 09:51:28 +0300 (Thu, 04 May 2017) $
#$Revision: 195986 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/58/4345819.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_4345819
loop_
_publ_author_name
'Deka, Hemanta'
'Ghosh, Somnath'
'Gogoi, Kuldeep'
'Saha, Soumen'
'Mondal, Biplab'
_publ_section_title
;
 Nitric Oxide Reactivity of a Cu(II) Complex of an Imidazole-Based Ligand:
 Aromatic C-Nitrosation Followed by the Formation of
 N-Nitrosohydroxylaminato Complex.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5034
_journal_page_last               5040
_journal_paper_doi               10.1021/acs.inorgchem.7b00069
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C38 H52 Cu N10 O8'
_chemical_formula_weight         840.44
_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                65.122(9)
_cell_angle_beta                 76.964(8)
_cell_angle_gamma                78.346(7)
_cell_formula_units_Z            1
_cell_length_a                   8.4863(8)
_cell_length_b                   10.9805(10)
_cell_length_c                   12.8436(12)
_cell_measurement_reflns_used    7349
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.0
_cell_volume                     1049.98(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7349
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'face installed'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             443
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0497
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1653
_reflns_number_gt                3139
_reflns_number_total             3797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7b00069_si_004.cif
_cod_data_source_block           Complex3
_cod_original_cell_volume        1049.99(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4345819
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
Cu1 Cu 0.5000 1.0000 1.0000 0.0211(2) Uani 1 2 d S
O2 O 0.7530(3) 0.5699(3) 0.6181(2) 0.0424(7) Uani 1 1 d .
N2 N 0.2884(3) 1.2173(3) 0.7034(2) 0.0269(6) Uani 1 1 d .
H2N H 0.2490 1.2902 0.6517 0.032 Uiso 1 1 calc R
N3 N 0.3923(3) 0.8340(2) 1.0461(2) 0.0214(6) Uani 1 1 d .
O1 O 0.7230(3) 0.9215(2) 0.88973(19) 0.0298(5) Uani 1 1 d .
N4 N 0.2974(3) 0.6387(3) 1.1361(2) 0.0277(6) Uani 1 1 d .
H4N H 0.2603 0.5682 1.1915 0.033 Uiso 1 1 calc R
C4 C 0.3308(4) 1.0934(3) 0.6948(3) 0.0251(7) Uani 1 1 d .
C17 C 0.8259(4) 0.7008(3) 0.6907(3) 0.0277(7) Uani 1 1 d .
C7 C 0.4416(4) 0.8568(3) 0.8351(3) 0.0220(7) Uani 1 1 d .
H7 H 0.3797 0.8250 0.7976 0.026 Uiso 1 1 calc R
N5 N 0.8695(4) 0.6202(3) 0.6319(2) 0.0325(7) Uani 1 1 d .
C10 C 0.2951(4) 0.5653(3) 0.9744(3) 0.0337(8) Uani 1 1 d .
H10A H 0.3229 0.4739 1.0265 0.051 Uiso 1 1 calc R
H10B H 0.3587 0.5809 0.8989 0.051 Uiso 1 1 calc R
H10C H 0.1814 0.5799 0.9687 0.051 Uiso 1 1 calc R
C11 C 0.3334(4) 0.7455(3) 1.1491(3) 0.0234(7) Uani 1 1 d .
N1 N 0.3819(3) 1.0790(2) 0.8637(2) 0.0206(6) Uani 1 1 d .
C13 C 0.1207(4) 0.7805(4) 1.3078(3) 0.0377(9) Uani 1 1 d .
H13A H 0.0714 0.8596 1.2508 0.056 Uiso 1 1 calc R
H13B H 0.1066 0.7932 1.3790 0.056 Uiso 1 1 calc R
H13C H 0.0699 0.7034 1.3214 0.056 Uiso 1 1 calc R
C16 C 0.9512(4) 0.7462(4) 0.7149(3) 0.0360(9) Uani 1 1 d .
H16 H 1.0588 0.7246 0.6855 0.043 Uiso 1 1 calc R
C5 C 0.3121(5) 1.0719(4) 0.5912(3) 0.0383(9) Uani 1 1 d .
H5C H 0.2043 1.1082 0.5729 0.057 Uiso 1 1 calc R
H5B H 0.3292 0.9768 0.6078 0.057 Uiso 1 1 calc R
H6A H 0.3907 1.1169 0.5261 0.057 Uiso 1 1 calc R
C1 C 0.0979(4) 1.3552(4) 0.8739(3) 0.0398(9) Uani 1 1 d .
H1C H 0.0497 1.3831 0.8053 0.060 Uiso 1 1 calc R
H1A H 0.0772 1.4276 0.9003 0.060 Uiso 1 1 calc R
H1B H 0.0513 1.2775 0.9337 0.060 Uiso 1 1 calc R
C12 C 0.3025(4) 0.7572(3) 1.2635(3) 0.0279(7) Uani 1 1 d .
H12A H 0.3549 0.8317 1.2563 0.034 Uiso 1 1 calc R
H12B H 0.3507 0.6750 1.3199 0.034 Uiso 1 1 calc R
C3 C 0.3187(4) 1.2056(3) 0.8059(3) 0.0225(7) Uani 1 1 d .
C6 C 0.3878(3) 1.0080(3) 0.7954(3) 0.0212(7) Uani 1 1 d .
C8 C 0.3884(3) 0.7823(3) 0.9648(3) 0.0206(6) Uani 1 1 d .
C9 C 0.3299(3) 0.6607(3) 1.0195(3) 0.0246(7) Uani 1 1 d .
C14 C 0.7505(4) 0.8579(3) 0.8264(3) 0.0251(7) Uani 1 1 d .
C15 C 0.9184(4) 0.8210(4) 0.7803(3) 0.0333(8) Uani 1 1 d .
H15 H 1.0036 0.8489 0.7960 0.040 Uiso 1 1 calc R
C18 C 0.6598(4) 0.7411(3) 0.7315(3) 0.0266(7) Uani 1 1 d .
H18 H 0.5765 0.7135 0.7134 0.032 Uiso 1 1 calc R
C2 C 0.2798(4) 1.3195(3) 0.8462(3) 0.0267(7) Uani 1 1 d .
H2B H 0.3267 1.3982 0.7861 0.032 Uiso 1 1 calc R
H2A H 0.3286 1.2940 0.9150 0.032 Uiso 1 1 calc R
C19 C 0.6204(4) 0.8169(3) 0.7946(3) 0.0239(7) Uani 1 1 d .
O4 O 0.1902(3) 0.4975(3) 0.5653(2) 0.0338(6) Uani 1 1 d G
H2O4 H 0.1055 0.5482 0.5791 0.051 Uiso 1 1 d G
H1O4 H 0.1833 0.4808 0.5077 0.051 Uiso 1 1 d G
O3 O 0.3920(5) 0.6474(4) 0.6130(4) 0.0709(11) Uani 1 1 d .
H2O3 H 0.356(5) 0.600(5) 0.594(4) 0.052(14) Uiso 1 1 d .
H1O3 H 0.488(7) 0.641(5) 0.585(5) 0.074(19) Uiso 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'
Cu Cu 0.3201 1.2651 '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 Cu1 N1 180.00(10) 2_677 .
N1 Cu1 N3 85.84(10) 2_677 2_677
N1 Cu1 N3 94.16(10) . 2_677
N1 Cu1 N3 94.16(10) 2_677 .
N1 Cu1 N3 85.83(10) . .
N3 Cu1 N3 179.999(1) 2_677 .
N1 Cu1 O1 89.61(9) 2_677 2_677
N1 Cu1 O1 90.39(9) . 2_677
N3 Cu1 O1 91.45(9) 2_677 2_677
N3 Cu1 O1 88.55(9) . 2_677
N1 Cu1 O1 90.39(9) 2_677 .
N1 Cu1 O1 89.61(9) . .
N3 Cu1 O1 88.55(9) 2_677 .
N3 Cu1 O1 91.45(9) . .
O1 Cu1 O1 180.00(10) 2_677 .
C3 N2 C4 109.1(3) . .
C11 N3 C8 106.7(2) . .
C11 N3 Cu1 132.0(2) . .
C8 N3 Cu1 120.87(19) . .
C14 O1 Cu1 138.7(2) . .
C11 N4 C9 109.3(3) . .
C6 C4 N2 105.4(3) . .
C6 C4 C5 132.0(3) . .
N2 C4 C5 122.5(3) . .
N5 C17 C16 117.3(3) . .
N5 C17 C18 124.0(3) . .
C16 C17 C18 118.7(3) . .
C8 C7 C6 111.8(2) . .
C8 C7 C19 113.0(3) . .
C6 C7 C19 115.4(2) . .
O2 N5 C17 116.8(3) . .
N3 C11 N4 109.3(3) . .
N3 C11 C12 128.0(3) . .
N4 C11 C12 122.7(3) . .
C3 N1 C6 106.8(3) . .
C3 N1 Cu1 131.1(2) . .
C6 N1 Cu1 120.6(2) . .
C15 C16 C17 121.3(3) . .
C11 C12 C13 112.3(3) . .
N1 C3 N2 109.5(3) . .
N1 C3 C2 127.2(3) . .
N2 C3 C2 123.3(3) . .
C4 C6 N1 109.2(3) . .
C4 C6 C7 127.8(3) . .
N1 C6 C7 122.9(3) . .
C9 C8 N3 109.8(3) . .
C9 C8 C7 127.3(3) . .
N3 C8 C7 122.9(2) . .
C8 C9 N4 104.9(3) . .
C8 C9 C10 132.0(3) . .
N4 C9 C10 123.0(3) . .
O1 C14 C15 119.8(3) . .
O1 C14 C19 122.7(3) . .
C15 C14 C19 117.5(3) . .
C16 C15 C14 120.6(3) . .
C19 C18 C17 122.5(3) . .
C3 C2 C1 111.6(3) . .
C18 C19 C14 119.3(3) . .
C18 C19 C7 120.0(3) . .
C14 C19 C7 120.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.996(2) 2_677
Cu1 N1 1.996(3) .
Cu1 N3 2.007(2) 2_677
Cu1 N3 2.007(2) .
Cu1 O1 2.343(2) 2_677
Cu1 O1 2.343(2) .
O2 N5 1.303(4) .
N2 C3 1.347(4) .
N2 C4 1.380(4) .
N3 C11 1.327(4) .
N3 C8 1.391(4) .
O1 C14 1.236(4) .
N4 C11 1.353(4) .
N4 C9 1.383(4) .
C4 C6 1.365(4) .
C4 C5 1.492(4) .
C17 N5 1.339(4) .
C17 C16 1.404(5) .
C17 C18 1.438(4) .
C7 C8 1.520(4) .
C7 C6 1.520(4) .
C7 C19 1.527(4) .
C10 C9 1.494(4) .
C11 C12 1.489(4) .
N1 C3 1.334(4) .
N1 C6 1.386(4) .
C13 C12 1.528(4) .
C16 C15 1.357(5) .
C1 C2 1.513(5) .
C3 C2 1.497(4) .
C8 C9 1.359(4) .
C14 C15 1.460(4) .
C14 C19 1.466(5) .
C18 C19 1.340(4) .
