#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:51:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179993 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/87/7028755.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_7028755
loop_
_publ_author_name
'Mulyana, Yanyan'
'Alley, Kerwyn G.'
'Davies, Kristian M.'
'Abrahams, Brendan F.'
'Moubaraki, Boujemaa'
'Murray, Keith S.'
'Boskovic, Colette'
_publ_section_title
;
 Dinuclear cobalt(ii) and cobalt(iii) complexes of bis-bidentate
 napthoquinone ligands.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2499
_journal_page_last               2511
_journal_paper_doi               10.1039/c3dt52811a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C50 H36 N2 O15'
_chemical_formula_weight         904.81
_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                68.347(4)
_cell_angle_beta                 81.383(4)
_cell_angle_gamma                76.412(4)
_cell_formula_units_Z            1
_cell_length_a                   7.277(2)
_cell_length_b                   11.987(3)
_cell_length_c                   12.828(3)
_cell_measurement_reflns_used    2874
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.9
_cell_volume                     1008.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0960
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5325
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.9900
_exptl_absorpt_correction_T_min  0.9557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         3493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0744
_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)+(0.1064P)²+0.6274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.2009
_reflns_number_gt                3254
_reflns_number_total             3493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52811a.txt
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7028755
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
O5 O 0.2376(3) 0.91352(17) 0.66978(16) 0.0293(5) Uani 1 1 d .
O1 O 0.0541(3) 0.67201(19) 1.05945(17) 0.0345(5) Uani 1 1 d .
O4 O 0.2297(3) 1.01801(17) 0.44712(16) 0.0313(5) Uani 1 1 d .
N1 N 0.2981(3) 0.1380(2) 0.6031(2) 0.0256(5) Uani 1 1 d .
O2 O 0.0480(3) 0.82128(18) 0.84955(17) 0.0312(5) Uani 1 1 d .
O6 O 0.0669(3) 0.57356(17) 0.64032(16) 0.0282(5) Uani 1 1 d .
C20 C 0.1362(3) 0.6563(2) 0.4051(2) 0.0251(6) Uani 1 1 d .
H008 H 0.1096 0.5763 0.4398 0.030 Uiso 1 1 calc R
C13 C 0.1886(3) 0.7285(2) 0.6632(2) 0.0233(6) Uani 1 1 d .
C16 C 0.1872(3) 0.8424(2) 0.4181(2) 0.0233(6) Uani 1 1 d .
C14 C 0.1321(3) 0.6676(2) 0.5966(2) 0.0233(6) Uani 1 1 d .
C3 C 0.2085(3) 0.6588(2) 0.7838(2) 0.0233(6) Uani 1 1 d .
C11 C 0.2070(3) 0.9119(2) 0.4890(2) 0.0251(6) Uani 1 1 d .
C17 C 0.2053(4) 0.8931(3) 0.3018(2) 0.0284(6) Uani 1 1 d .
H014 H 0.2268 0.9743 0.2662 0.034 Uiso 1 1 calc R
C5 C 0.3298(4) 0.4536(3) 0.9356(2) 0.0254(6) Uani 1 1 d .
C10 C 0.4278(4) 0.3335(3) 0.9649(2) 0.0300(6) Uani 1 1 d .
H016 H 0.4955 0.3035 0.9083 0.036 Uiso 1 1 calc R
C8 C 0.3294(4) 0.3006(3) 1.1593(2) 0.0368(7) Uani 1 1 d .
H017 H 0.3285 0.2477 1.2357 0.044 Uiso 1 1 calc R
C15 C 0.1523(3) 0.7230(2) 0.4711(2) 0.0233(6) Uani 1 1 d .
C1 C 0.1358(4) 0.6278(3) 0.9889(2) 0.0276(6) Uani 1 1 d .
C21 C 0.2864(4) 0.1609(3) 0.6984(2) 0.0286(6) Uani 1 1 d .
H020 H 0.2558 0.1015 0.7682 0.034 Uiso 1 1 calc R
C2 C 0.1353(4) 0.7056(3) 0.8673(2) 0.0271(6) Uani 1 1 d .
C19 C 0.1589(4) 0.7061(3) 0.2892(2) 0.0293(6) Uani 1 1 d .
H023 H 0.1518 0.6592 0.2448 0.035 Uiso 1 1 calc R
C6 C 0.2328(4) 0.4978(3) 1.0197(2) 0.0269(6) Uani 1 1 d .
C24 C 0.3714(4) 0.3306(3) 0.4957(2) 0.0285(6) Uani 1 1 d .
H025 H 0.4002 0.3889 0.4248 0.034 Uiso 1 1 calc R
C18 C 0.1918(4) 0.8243(3) 0.2376(2) 0.0324(7) Uani 1 1 d .
H026 H 0.2053 0.8584 0.1579 0.039 Uiso 1 1 calc R
C12 C 0.2097(4) 0.8488(2) 0.6143(2) 0.0248(6) Uani 1 1 d .
C23 C 0.3631(4) 0.3558(2) 0.5923(3) 0.0292(6) Uani 1 1 d .
H028 H 0.3877 0.4316 0.5888 0.035 Uiso 1 1 calc R
C9 C 0.4275(4) 0.2571(3) 1.0763(3) 0.0351(7) Uani 1 1 d .
H029 H 0.4945 0.1747 1.0959 0.042 Uiso 1 1 calc R
C25 C 0.3375(4) 0.2197(2) 0.5023(2) 0.0266(6) Uani 1 1 d .
H030 H 0.3420 0.2013 0.4359 0.032 Uiso 1 1 calc R
C22 C 0.3188(4) 0.2706(3) 0.6954(3) 0.0308(6) Uani 1 1 d .
H031 H 0.3109 0.2877 0.7628 0.037 Uiso 1 1 calc R
C7 C 0.2331(4) 0.4205(3) 1.1315(2) 0.0311(6) Uani 1 1 d .
H033 H 0.1669 0.4501 1.1887 0.037 Uiso 1 1 calc R
O3 O 0.4289(3) 0.49929(17) 0.74345(16) 0.0287(5) Uani 1 1 d .
C4 C 0.3271(3) 0.5347(2) 0.8150(2) 0.0230(6) Uani 1 1 d .
O8 O 0.8661(4) 0.9244(2) 0.0357(2) 0.0455(6) Uani 1 1 d .
O7 O 0.4944(7) 0.9758(5) 0.0495(5) 0.0578(14) Uani 0.50 1 d P
H100 H 0.286(5) 0.061(4) 0.608(3) 0.046(10) Uiso 1 1 d .
H101 H 0.093(6) 0.865(4) 0.780(4) 0.059(12) Uiso 1 1 d .
H102 H 0.903(7) 0.875(5) 0.009(4) 0.069(15) 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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C21 N1 C25 122.3(2)
C19 C20 C15 120.3(3)
C12 C13 C14 120.1(2)
C12 C13 C3 122.7(2)
C14 C13 C3 117.1(2)
C17 C16 C15 120.5(3)
C17 C16 C11 120.9(2)
C15 C16 C11 118.6(2)
O6 C14 C13 122.2(2)
O6 C14 C15 119.3(2)
C13 C14 C15 118.5(2)
C2 C3 C13 123.9(2)
C2 C3 C4 118.5(2)
C13 C3 C4 117.5(2)
O4 C11 C16 121.3(2)
O4 C11 C12 119.4(2)
C16 C11 C12 119.3(2)
C16 C17 C18 119.5(3)
C10 C5 C6 119.5(3)
C10 C5 C4 120.1(2)
C6 C5 C4 120.4(2)
C9 C10 C5 120.4(3)
C7 C8 C9 120.2(3)
C20 C15 C16 119.0(2)
C20 C15 C14 120.1(2)
C16 C15 C14 120.9(2)
O1 C1 C6 122.1(2)
O1 C1 C2 119.5(3)
C6 C1 C2 118.3(2)
N1 C21 C22 120.0(3)
O2 C2 C3 124.4(3)
O2 C2 C1 113.2(2)
C3 C2 C1 122.3(3)
C20 C19 C18 120.3(3)
C7 C6 C5 119.8(3)
C7 C6 C1 120.7(3)
C5 C6 C1 119.5(2)
C23 C24 C25 119.3(3)
C19 C18 C17 120.4(3)
O5 C12 C13 123.9(2)
O5 C12 C11 115.6(2)
C13 C12 C11 120.5(2)
C24 C23 C22 120.0(3)
C10 C9 C8 120.0(3)
N1 C25 C24 119.6(3)
C21 C22 C23 118.8(3)
C8 C7 C6 120.1(3)
O3 C4 C3 120.7(2)
O3 C4 C5 119.7(2)
C3 C4 C5 119.6(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O5 C12 1.295(3) .
O1 C1 1.224(3) .
O4 C11 1.225(3) .
N1 C21 1.336(4) .
N1 C25 1.341(4) .
O2 C2 1.332(3) .
O6 C14 1.231(3) .
C20 C19 1.382(4) .
C20 C15 1.394(4) .
C13 C12 1.379(4) .
C13 C14 1.463(4) .
C13 C3 1.472(4) .
C16 C17 1.386(4) .
C16 C15 1.406(4) .
C16 C11 1.483(4) .
C14 C15 1.496(4) .
C3 C2 1.371(4) .
C3 C4 1.476(4) .
C11 C12 1.504(4) .
C17 C18 1.389(4) .
C5 C10 1.386(4) .
C5 C6 1.401(4) .
C5 C4 1.493(4) .
C10 C9 1.384(4) .
C8 C7 1.381(5) .
C8 C9 1.387(4) .
C1 C6 1.481(4) .
C1 C2 1.493(4) .
C21 C22 1.375(4) .
C19 C18 1.387(4) .
C6 C7 1.391(4) .
C24 C23 1.370(4) .
C24 C25 1.378(4) .
C23 C22 1.388(4) .
O3 C4 1.228(3) .
O7 O7 1.184(11) 2_675
