#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:17:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179916 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/11/7021179.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_7021179
loop_
_publ_author_name
'Kumar, Pankaj'
'Kalita, Apurba'
'Mondal, Biplab'
_publ_section_title
;
 Nitric oxide reactivity of Cu(ii) complexes of tetra- and pentadentate
 ligands: structural influence in deciding the reduction pathway.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5731
_journal_page_last               5739
_journal_paper_doi               10.1039/c3dt32580f
_journal_volume                  42
_journal_year                    2013
_chemical_compound_source        Synthesised
_chemical_formula_moiety         'C30 H36 Cl3 Cu2 N8 O12, O'
_chemical_formula_sum            'C30 H36 Cl3 Cu2 N8 O13'
_chemical_formula_weight         950.12
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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            4
_cell_length_a                   13.6944(4)
_cell_length_b                   26.3827(8)
_cell_length_c                   11.2946(3)
_cell_measurement_reflns_used    8877
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     4080.7(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1019
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            42599
_diffrn_reflns_theta_full        23.18
_diffrn_reflns_theta_max         23.18
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.308
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADBAS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1940
_exptl_crystal_recrystallization_method Acetonitrile
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.224
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.664
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         2968
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.673
_refine_ls_R_factor_all          0.1461
_refine_ls_R_factor_gt           0.1303
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3822
_refine_ls_wR_factor_ref         0.3940
_reflns_number_gt                2197
_reflns_number_total             2968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32580f.txt
_cod_data_source_block           2
_cod_database_code               7021179
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.26087(9) 0.61615(5) 0.04737(11) 0.0560(7) Uani 1 1 d .
Cl1 Cl 0.3240(2) 0.48039(12) 0.0482(3) 0.0729(11) Uani 1 1 d D
Cl2 Cl 0.2097(4) 0.7500 0.0655(5) 0.0793(14) Uani 1 2 d SD
N4 N 0.3194(6) 0.6389(3) 0.1986(7) 0.057(2) Uani 1 1 d .
N1 N 0.1376(6) 0.5823(3) 0.0962(7) 0.053(2) Uani 1 1 d .
N3 N 0.3900(8) 0.6381(6) -0.0172(9) 0.101(4) Uani 1 1 d .
N2 N 0.1992(9) 0.6089(6) -0.1101(9) 0.118(5) Uani 1 1 d D
C4 C -0.0231(7) 0.5619(5) 0.0372(10) 0.063(3) Uani 1 1 d .
H4 H -0.0704 0.5628 -0.0219 0.076 Uiso 1 1 calc R
C1 C 0.1206(8) 0.5581(4) 0.1981(9) 0.063(3) Uani 1 1 d .
H1 H 0.1714 0.5554 0.2524 0.076 Uiso 1 1 calc R
C6 C 0.0939(10) 0.6088(5) -0.1018(11) 0.075(3) Uani 1 1 d .
H6A H 0.0658 0.5901 -0.1674 0.090 Uiso 1 1 calc R
H6B H 0.0690 0.6432 -0.1037 0.090 Uiso 1 1 calc R
C2 C 0.0327(8) 0.5371(4) 0.2268(11) 0.070(3) Uani 1 1 d .
H2 H 0.0219 0.5212 0.2991 0.084 Uiso 1 1 calc R
C11 C 0.4120(8) 0.6529(4) 0.1923(9) 0.057(3) Uani 1 1 d .
C5 C 0.0677(8) 0.5832(4) 0.0165(9) 0.055(3) Uani 1 1 d .
C3 C -0.0430(9) 0.5411(4) 0.1367(14) 0.079(4) Uani 1 1 d .
H3 H -0.1053 0.5287 0.1514 0.094 Uiso 1 1 calc R
C8 C 0.3467(11) 0.6288(5) -0.2265(12) 0.084(4) Uani 1 1 d .
H8A H 0.3634 0.5974 -0.2665 0.101 Uiso 1 1 calc R
H8B H 0.3631 0.6559 -0.2810 0.101 Uiso 1 1 calc R
C10 C 0.4621(9) 0.6421(5) 0.0717(11) 0.075(3) Uani 1 1 d .
H10A H 0.5070 0.6693 0.0525 0.090 Uiso 1 1 calc R
H10B H 0.4989 0.6107 0.0764 0.090 Uiso 1 1 calc R
C12 C 0.4618(10) 0.6758(4) 0.2843(13) 0.074(3) Uani 1 1 d .
H12 H 0.5268 0.6852 0.2759 0.089 Uiso 1 1 calc R
C15 C 0.2727(9) 0.6488(5) 0.3032(10) 0.067(3) Uani 1 1 d .
H15 H 0.2072 0.6399 0.3103 0.081 Uiso 1 1 calc R
C14 C 0.3189(12) 0.6719(5) 0.4005(10) 0.086(4) Uani 1 1 d .
H14 H 0.2859 0.6784 0.4709 0.103 Uiso 1 1 calc R
C9 C 0.4116(12) 0.6331(9) -0.1331(13) 0.131(7) Uani 1 1 d .
H9A H 0.4535 0.6035 -0.1383 0.158 Uiso 1 1 calc R
H9B H 0.4526 0.6620 -0.1523 0.158 Uiso 1 1 calc R
C13 C 0.4139(14) 0.6841(5) 0.3861(15) 0.093(5) Uani 1 1 d .
H13 H 0.4473 0.6988 0.4490 0.112 Uiso 1 1 calc R
O1 O 0.265(2) 0.4761(8) 0.148(3) 0.35(2) Uani 1 1 d D
O2 O 0.3439(10) 0.5292(5) 0.0775(14) 0.148(5) Uani 1 1 d D
O3 O 0.4058(10) 0.4498(5) 0.0531(15) 0.172(6) Uani 1 1 d D
O5 O 0.1624(8) 0.7045(4) 0.0532(11) 0.124(4) Uani 1 1 d D
O8 O 0.6051(19) 0.7500 0.880(2) 0.220(14) Uani 1 2 d S
C7 C 0.2428(11) 0.6291(9) -0.2170(14) 0.141(10) Uani 1 1 d D
H7A H 0.2167 0.6102 -0.2836 0.170 Uiso 1 1 calc R
H7B H 0.2209 0.6639 -0.2257 0.170 Uiso 1 1 calc R
O6 O 0.3093(11) 0.7500 0.085(2) 0.155(8) Uani 1 2 d SD
O4 O 0.316(3) 0.4987(15) -0.0684(17) 0.42(3) Uani 1 1 d D
O7 O 0.202(2) 0.7500 0.1940(16) 0.205(11) Uani 1 2 d SD
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'
Cl Cl 0.1484 0.1585 '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
N2 Cu1 N4 167.9(5) .
N2 Cu1 N1 81.0(4) .
N4 Cu1 N1 103.9(3) .
N2 Cu1 N3 94.5(4) .
N4 Cu1 N3 82.4(4) .
N1 Cu1 N3 169.4(5) .
O2 Cl1 O3 112.4(10) .
O2 Cl1 O1 89.8(13) .
O3 Cl1 O1 112.8(14) .
O2 Cl1 O4 85.3(16) .
O3 Cl1 O4 108(2) .
O1 Cl1 O4 138(3) .
O5 Cl2 O5 122.1(11) 7_575
O5 Cl2 O6 118.9(6) 7_575
O5 Cl2 O6 118.9(6) .
O5 Cl2 O7 93.7(8) 7_575
O5 Cl2 O7 93.7(8) .
O6 Cl2 O7 85.2(15) .
C11 N4 C15 116.1(9) .
C11 N4 Cu1 115.3(7) .
C15 N4 Cu1 127.8(8) .
C5 N1 C1 118.1(9) .
C5 N1 Cu1 114.9(7) .
C1 N1 Cu1 127.0(7) .
C9 N3 C10 123.0(12) .
C9 N3 Cu1 121.3(10) .
C10 N3 Cu1 112.4(8) .
C6 N2 C7 117.7(11) .
C6 N2 Cu1 111.6(8) .
C7 N2 Cu1 122.6(9) .
C3 C4 C5 120.8(11) .
N1 C1 C2 123.6(11) .
N2 C6 C5 106.8(10) .
C1 C2 C3 115.6(11) .
N4 C11 C12 123.7(11) .
N4 C11 C10 114.8(9) .
C12 C11 C10 121.5(11) .
N1 C5 C4 122.1(10) .
N1 C5 C6 115.6(9) .
C4 C5 C6 122.2(10) .
C4 C3 C2 119.6(11) .
C9 C8 C7 125.6(13) .
N3 C10 C11 109.2(9) .
C13 C12 C11 118.3(12) .
N4 C15 C14 123.1(12) .
C13 C14 C15 116.3(12) .
N3 C9 C8 127.4(14) .
C12 C13 C14 122.4(12) .
C8 C7 N2 118.1(14) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.978(10) .
Cu1 N4 1.979(8) .
Cu1 N1 1.988(8) .
Cu1 N3 1.999(10) .
Cl1 O2 1.356(12) .
Cl1 O3 1.383(11) .
Cl1 O1 1.393(14) .
Cl1 O4 1.407(15) .
Cl2 O5 1.371(10) 7_575
Cl2 O5 1.371(10) .
Cl2 O6 1.381(14) .
Cl2 O7 1.456(17) .
N4 C11 1.323(14) .
N4 C15 1.370(14) .
N1 C5 1.315(13) .
N1 C1 1.337(13) .
N3 C9 1.349(17) .
N3 C10 1.412(16) .
N2 C6 1.446(18) .
N2 C7 1.449(15) .
C4 C3 1.279(17) .
C4 C5 1.384(15) .
C1 C2 1.364(14) .
C6 C5 1.540(16) .
C2 C3 1.457(17) .
C11 C12 1.382(15) .
C11 C10 1.552(16) .
C8 C9 1.38(2) .
C8 C7 1.428(19) .
C12 C13 1.34(2) .
C15 C14 1.407(18) .
C14 C13 1.35(2) .
