#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:46:40 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/78/7047876.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_7047876
loop_
_publ_author_name
'Papanikolaou, Michael G.'
'Hadjithoma, Sofia'
'Chatzikypraiou, Dimitra S.'
'Papaioannou, Dionysios'
'Drouza, Chryssoula'
'Tsipis, Athanassios C.'
'Miras, Haralampos N.'
'Keramidas, Anastasios D.'
'Kabanos, Themistoklis A.'
_publ_section_title
;
 Investigation of dioxygen activation by copper(ii)-iminate/aminate
 complexes.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16242
_journal_page_last               16254
_journal_paper_doi               10.1039/c8dt03137a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C40 H26 Cu2 N8 O6'
_chemical_formula_sum            'C40 H26 Cu2 N8 O6'
_chemical_formula_weight         841.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2018/3
_audit_update_record
;
2018-10-18 deposited with the CCDC.
2018-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                114.711(4)
_cell_angle_beta                 98.049(5)
_cell_angle_gamma                106.462(5)
_cell_formula_units_Z            1
_cell_length_a                   9.4219(6)
_cell_length_b                   10.0037(7)
_cell_length_c                   10.3783(7)
_cell_measurement_reflns_used    3690
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.587
_cell_measurement_theta_min      2.262
_cell_volume                     813.82(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Apex II Quazar CCD'
_diffrn_measurement_method       'ω & φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14401
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.395
_diffrn_reflns_theta_min         2.262
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4705
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0409P)²+1.3605P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2558
_reflns_number_total             3319
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03137a2.cif
_cod_data_source_block           shelx_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7047874--7047877.cif.'
_cod_original_cell_volume        813.82(10)
_cod_database_code               7047876
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.852
_shelx_estimated_absorpt_t_max   0.898
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C1 C 0.7981(4) 0.1005(4) 0.2903(4) 0.0255(8) Uani 1 1 d . .
H1 H 0.823241 0.085672 0.373958 0.031 Uiso 1 1 calc R U
C2 C 0.8851(4) 0.0748(4) 0.1921(4) 0.0283(9) Uani 1 1 d . .
H2 H 0.968693 0.042592 0.207717 0.034 Uiso 1 1 calc R U
C3 C 0.8481(4) 0.0968(4) 0.0713(4) 0.0288(9) Uani 1 1 d . .
H3 H 0.907118 0.080988 0.003019 0.035 Uiso 1 1 calc R U
C4 C 0.7249(4) 0.1419(4) 0.0495(4) 0.0261(8) Uani 1 1 d . .
H4 H 0.697740 0.156816 -0.033741 0.031 Uiso 1 1 calc R U
C5 C 0.6419(4) 0.1648(4) 0.1514(4) 0.0207(7) Uani 1 1 d . .
C6 C 0.5074(4) 0.2177(4) 0.1377(4) 0.0220(8) Uani 1 1 d . .
C7 C 0.3448(4) 0.3104(4) 0.2920(4) 0.0219(8) Uani 1 1 d . .
C8 C 0.2663(4) 0.3597(4) 0.2065(4) 0.0260(8) Uani 1 1 d . .
H8 H 0.277256 0.337688 0.110880 0.031 Uiso 1 1 calc R U
C9 C 0.1735(4) 0.4402(4) 0.2616(4) 0.0265(8) Uani 1 1 d . .
H9 H 0.119947 0.472840 0.203079 0.032 Uiso 1 1 calc R U
C10 C 0.1570(4) 0.4743(4) 0.4011(4) 0.0269(8) Uani 1 1 d . .
H10 H 0.095595 0.533394 0.439112 0.032 Uiso 1 1 calc R U
C11 C 0.2297(4) 0.4224(4) 0.4856(4) 0.0247(8) Uani 1 1 d . .
H11 H 0.217140 0.445329 0.580835 0.030 Uiso 1 1 calc R U
C12 C 0.3216(4) 0.3362(4) 0.4313(4) 0.0208(7) Uani 1 1 d . .
C13 C 0.5965(3) 0.1625(4) 0.6584(3) 0.0104(6) Uani 1 1 d . .
C14 C 0.4873(4) 0.2171(4) 0.6990(4) 0.0235(8) Uani 1 1 d . .
H14 H 0.470155 0.222527 0.788750 0.028 Uiso 1 1 calc R U
C15 C 0.3938(4) 0.2680(4) 0.6261(4) 0.0210(7) Uani 1 1 d . .
C16 C 0.2679(4) 0.2939(4) 0.6976(4) 0.0215(8) Uani 1 1 d . .
C17 C 0.3032(5) 0.4185(4) 0.8381(4) 0.0278(8) Uani 1 1 d . .
H17 H 0.406463 0.493476 0.890731 0.033 Uiso 1 1 calc R U
C18 C 0.1836(5) 0.4308(5) 0.9001(4) 0.0325(10) Uani 1 1 d . .
H18 H 0.202382 0.516914 0.995293 0.039 Uiso 1 1 calc R U
C19 C 0.0368(5) 0.3163(5) 0.8214(5) 0.0329(9) Uani 1 1 d . .
H19 H -0.046906 0.321312 0.862251 0.039 Uiso 1 1 calc R U
C20 C 0.0128(5) 0.1935(5) 0.6819(4) 0.0318(9) Uani 1 1 d . .
H20 H -0.088637 0.114193 0.629180 0.038 Uiso 1 1 calc R U
N1 N 0.1258(4) 0.1812(4) 0.6178(3) 0.0271(7) Uani 1 1 d . .
N2 N 0.4080(3) 0.2811(3) 0.5072(3) 0.0196(6) Uani 1 1 d . .
N3 N 0.4526(3) 0.2422(3) 0.2553(3) 0.0195(6) Uani 1 1 d . .
N4 N 0.6799(3) 0.1455(3) 0.2712(3) 0.0211(6) Uani 1 1 d . .
O1 O 0.6590(3) 0.1058(3) 0.7276(3) 0.0326(6) Uani 1 1 d . .
O2 O 0.6427(3) 0.1579(3) 0.5441(3) 0.0232(5) Uani 1 1 d . .
O3 O 0.4640(3) 0.2344(3) 0.0294(3) 0.0268(6) Uani 1 1 d . .
Cu1 Cu 0.54524(5) 0.20021(5) 0.40089(5) 0.02250(15) 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'
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
N4 C1 C2 122.0(3)
N4 C1 H1 119.0
C2 C1 H1 119.0
C3 C2 C1 118.7(3)
C3 C2 H2 120.7
C1 C2 H2 120.7
C2 C3 C4 119.8(3)
C2 C3 H3 120.1
C4 C3 H3 120.1
C5 C4 C3 118.7(3)
C5 C4 H4 120.7
C3 C4 H4 120.7
N4 C5 C4 121.4(3)
N4 C5 C6 116.5(3)
C4 C5 C6 122.1(3)
O3 C6 N3 129.1(3)
O3 C6 C5 120.0(3)
N3 C6 C5 110.9(3)
N3 C7 C8 125.2(3)
N3 C7 C12 114.9(3)
C8 C7 C12 119.8(3)
C9 C8 C7 119.8(3)
C9 C8 H8 120.1
C7 C8 H8 120.1
C8 C9 C10 120.9(3)
C8 C9 H9 119.6
C10 C9 H9 119.6
C9 C10 C11 120.2(3)
C9 C10 H10 119.9
C11 C10 H10 119.9
C10 C11 C12 120.4(3)
C10 C11 H11 119.8
C12 C11 H11 119.8
C11 C12 C7 118.7(3)
C11 C12 N2 126.8(3)
C7 C12 N2 114.3(3)
O1 C13 O2 115.3(3)
O1 C13 C14 120.9(3)
O2 C13 C14 123.7(3)
C13 C14 C15 128.6(3)
C13 C14 H14 115.7
C15 C14 H14 115.7
N2 C15 C14 124.8(3)
N2 C15 C16 124.8(3)
C14 C15 C16 110.3(3)
N1 C16 C17 124.5(3)
N1 C16 C15 114.5(3)
C17 C16 C15 120.9(3)
C16 C17 C18 117.9(4)
C16 C17 H17 121.0
C18 C17 H17 121.0
C19 C18 C17 118.9(4)
C19 C18 H18 120.6
C17 C18 H18 120.6
C18 C19 C20 119.1(3)
C18 C19 H19 120.4
C20 C19 H19 120.4
N1 C20 C19 123.1(4)
N1 C20 H20 118.4
C19 C20 H20 118.4
C20 N1 C16 116.4(3)
C15 N2 C12 127.7(3)
C15 N2 Cu1 120.5(2)
C12 N2 Cu1 111.5(2)
C6 N3 C7 127.6(3)
C6 N3 Cu1 117.8(2)
C7 N3 Cu1 114.4(2)
C1 N4 C5 119.4(3)
C1 N4 Cu1 129.5(2)
C5 N4 Cu1 111.0(2)
C13 O2 Cu1 124.4(2)
N3 Cu1 O2 178.35(11)
N3 Cu1 N2 84.81(11)
O2 Cu1 N2 96.77(11)
N3 Cu1 N4 83.84(11)
O2 Cu1 N4 94.55(11)
N2 Cu1 N4 167.59(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N4 1.334(4)
C1 C2 1.382(5)
C1 H1 0.9500
C2 C3 1.376(5)
C2 H2 0.9500
C3 C4 1.383(5)
C3 H3 0.9500
C4 C5 1.382(5)
C4 H4 0.9500
C5 N4 1.351(4)
C5 C6 1.516(5)
C6 O3 1.236(4)
C6 N3 1.347(4)
C7 N3 1.389(4)
C7 C8 1.402(5)
C7 C12 1.419(5)
C8 C9 1.377(5)
C8 H8 0.9500
C9 C10 1.385(5)
C9 H9 0.9500
C10 C11 1.386(5)
C10 H10 0.9500
C11 C12 1.401(5)
C11 H11 0.9500
C12 N2 1.424(4)
C13 O1 1.263(4)
C13 O2 1.308(4)
C13 C14 1.335(4)
C14 C15 1.413(5)
C14 H14 0.9500
C15 N2 1.315(4)
C15 C16 1.512(5)
C16 N1 1.343(5)
C16 C17 1.378(5)
C17 C18 1.384(5)
C17 H17 0.9500
C18 C19 1.377(6)
C18 H18 0.9500
C19 C20 1.386(6)
C19 H19 0.9500
C20 N1 1.340(5)
C20 H20 0.9500
N2 Cu1 1.946(3)
N3 Cu1 1.894(3)
N4 Cu1 1.995(3)
O2 Cu1 1.896(2)
