#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:14:05 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180253 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/39/7113951.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_7113951
loop_
_publ_author_name
'Timothy C. Davenport'
'Hyun S. Ahn'
'Micah S. Ziegler'
'T. Don Tilley'
_publ_section_title
;
 A molecular structural analog of proposed dinuclear active sites in
 cobalt-based water oxidation catalysts
;
_journal_name_full               Chem.Commun.
_journal_page_first              6326
_journal_paper_doi               10.1039/C3CC46865H
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C30 H26 Co2 F2 N6 O4 4+, 4(N O3 1-)'
_chemical_formula_sum            'C30 H26 Co2 F2 N10 O16'
_chemical_formula_weight         938.47
_chemical_name_common            '[Co2(u-OH)2(OH2)2(DPFN)][NO3]4'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 106.8370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.800(2)
_cell_length_b                   10.8131(8)
_cell_length_c                   12.7351(10)
_cell_measurement_reflns_used    4881
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.31
_cell_measurement_theta_min      2.49
_cell_volume                     3532.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3207
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         1.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.745212
_exptl_absorpt_correction_T_min  0.590955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0339P)²+4.6697P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0692
_reflns_number_gt                3100
_reflns_number_total             3207
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3cc46865h2.cif
_cod_data_source_block           '[Co2(u-OH)2(OH2)2(DPFN)][NO3]4'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7113951
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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
C1 C 0.59082(7) -0.01682(18) -0.20828(16) 0.0160(4) Uani 1 1 d .
C2 C 0.59310(8) -0.14627(19) -0.20681(18) 0.0202(4) Uani 1 1 d .
H2 H 0.6256 -0.1882 -0.1914 0.024 Uiso 1 1 calc R
C3 C 0.54767(8) -0.21032(19) -0.2280(2) 0.0230(4) Uani 1 1 d .
H3 H 0.5481 -0.2982 -0.2279 0.028 Uiso 1 1 calc R
C4 C 0.5000 -0.1464(3) -0.2500 0.0194(6) Uani 1 2 d S
C5 C 0.5000 -0.0150(2) -0.2500 0.0146(5) Uani 1 2 d S
C6 C 0.64171(7) 0.05700(18) -0.18378(16) 0.0164(4) Uani 1 1 d .
C7 C 0.64248(8) 0.1399(2) -0.27866(17) 0.0163(4) Uani 1 1 d .
C8 C 0.68049(8) 0.1352(2) -0.33212(18) 0.0203(4) Uani 1 1 d .
H8 H 0.7080 0.0766 -0.3117 0.024 Uiso 1 1 calc R
C9 C 0.67730(9) 0.2188(2) -0.41679(19) 0.0244(5) Uani 1 1 d .
H9 H 0.7027 0.2178 -0.4556 0.029 Uiso 1 1 calc R
C10 C 0.63670(9) 0.3035(2) -0.44409(19) 0.0258(5) Uani 1 1 d .
H10 H 0.6339 0.3610 -0.5019 0.031 Uiso 1 1 calc R
C11 C 0.60053(8) 0.3031(2) -0.3862(2) 0.0219(4) Uani 1 1 d .
H11 H 0.5727 0.3611 -0.4048 0.026 Uiso 1 1 calc R
C12 C 0.64880(8) 0.1334(2) -0.08065(17) 0.0174(4) Uani 1 1 d .
C13 C 0.69215(9) 0.1239(2) 0.00933(18) 0.0231(5) Uani 1 1 d .
H13 H 0.7194 0.0674 0.0101 0.028 Uiso 1 1 calc R
C14 C 0.69472(9) 0.1997(2) 0.09888(19) 0.0278(5) Uani 1 1 d .
H14 H 0.7244 0.1972 0.1616 0.033 Uiso 1 1 calc R
C15 C 0.65379(10) 0.2787(2) 0.0961(2) 0.0290(6) Uani 1 1 d .
H15 H 0.6545 0.3290 0.1576 0.035 Uiso 1 1 calc R
C16 C 0.61168(9) 0.2836(2) 0.0022(2) 0.0233(5) Uani 1 1 d .
H16 H 0.5837 0.3383 0.0000 0.028 Uiso 1 1 calc R
N1 N 0.54665(6) 0.04857(15) -0.22841(13) 0.0137(3) Uani 1 1 d .
N2 N 0.60358(7) 0.22272(16) -0.30407(15) 0.0157(4) Uani 1 1 d .
N3 N 0.60960(7) 0.21281(18) -0.08544(15) 0.0172(4) Uani 1 1 d .
O1 O 0.50205(7) 0.24653(13) -0.15159(12) 0.0155(3) Uani 1 1 d .
O2 O 0.55762(6) 0.40332(13) -0.21557(15) 0.0233(3) Uani 1 1 d .
F1 F 0.68251(4) -0.02599(11) -0.16640(10) 0.0216(3) Uani 1 1 d .
Co1 Co 0.554201(9) 0.22713(2) -0.22111(2) 0.01306(9) Uani 1 1 d .
H1A H 0.5025(13) 0.201(3) -0.109(2) 0.027(8) Uiso 1 1 d .
H2A H 0.5838(12) 0.441(3) -0.212(3) 0.042(8) Uiso 1 1 d .
H2B H 0.5420(16) 0.431(4) -0.167(3) 0.072(13) Uiso 1 1 d .
N4 N 0.67918(6) 0.47988(16) 0.34989(15) 0.0209(4) Uani 1 1 d .
O3 O 0.63264(5) 0.43984(14) 0.31201(14) 0.0257(4) Uani 1 1 d .
O4 O 0.68729(6) 0.59262(15) 0.34972(18) 0.0387(4) Uani 1 1 d .
O5 O 0.71440(6) 0.40460(17) 0.38588(19) 0.0420(5) Uani 1 1 d .
N5 N 0.5000 0.0000 0.0000 0.0423(8) Uani 1 2 d S
O6 O 0.4874(3) 0.1091(5) 0.0037(4) 0.0647(17) Uani 0.50 1 d P
O7 O 0.5254(2) 0.0886(6) 0.0132(4) 0.0558(14) Uani 0.50 1 d P
O8 O 0.55246(16) -0.0140(4) 0.0170(3) 0.0479(10) Uani 0.50 1 d P
N6 N 0.49829(13) 0.4774(2) 0.0439(2) 0.0604(7) Uani 0.50 1 d P
O9 O 0.54199(16) 0.4217(4) 0.1023(3) 0.0422(10) Uani 0.50 1 d P
O10 O 0.46235(14) 0.4772(4) 0.0556(4) 0.0479(13) Uani 0.50 1 d P
O11 O 0.49829(13) 0.4774(2) 0.0439(2) 0.0604(7) Uani 0.50 1 d P
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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 124.28(18) . .
N1 C1 C6 116.71(17) . .
C2 C1 C6 119.01(17) . .
C3 C2 C1 118.28(18) . .
C3 C2 H2 120.9 . .
C1 C2 H2 120.9 . .
C2 C3 C4 119.91(19) . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C3 C4 C3 121.1(3) 2_654 .
C3 C4 C5 119.43(13) 2_654 .
C3 C4 C5 119.43(13) . .
N1 C5 N1 120.4(2) . 2_654
N1 C5 C4 119.80(11) . .
N1 C5 C4 119.80(11) 2_654 .
F1 C6 C7 108.68(16) . .
F1 C6 C12 108.68(16) . .
C7 C6 C12 110.03(16) . .
F1 C6 C1 108.10(16) . .
C7 C6 C1 111.35(16) . .
C12 C6 C1 109.93(16) . .
N2 C7 C8 122.6(2) . .
N2 C7 C6 113.57(18) . .
C8 C7 C6 123.78(19) . .
C7 C8 C9 118.1(2) . .
C7 C8 H8 121.0 . .
C9 C8 H8 121.0 . .
C10 C9 C8 119.4(2) . .
C10 C9 H9 120.3 . .
C8 C9 H9 120.3 . .
C11 C10 C9 119.1(2) . .
C11 C10 H10 120.5 . .
C9 C10 H10 120.5 . .
N2 C11 C10 121.7(2) . .
N2 C11 H11 119.2 . .
C10 C11 H11 119.2 . .
N3 C12 C13 123.0(2) . .
N3 C12 C6 114.11(18) . .
C13 C12 C6 122.9(2) . .
C12 C13 C14 117.9(2) . .
C12 C13 H13 121.1 . .
C14 C13 H13 121.1 . .
C15 C14 C13 119.5(2) . .
C15 C14 H14 120.2 . .
C13 C14 H14 120.2 . .
C14 C15 C16 119.2(2) . .
C14 C15 H15 120.4 . .
C16 C15 H15 120.4 . .
N3 C16 C15 121.5(2) . .
N3 C16 H16 119.2 . .
C15 C16 H16 119.2 . .
C1 N1 C5 118.31(17) . .
C1 N1 Co1 116.25(12) . .
C5 N1 Co1 125.42(13) . .
C7 N2 C11 119.17(19) . .
C7 N2 Co1 119.73(15) . .
C11 N2 Co1 121.08(15) . .
C16 N3 C12 118.88(19) . .
C16 N3 Co1 122.34(16) . .
C12 N3 Co1 118.69(15) . .
Co1 O1 Co1 95.85(7) . 2_654
Co1 O1 H1A 115(3) . .
Co1 O1 H1A 114(3) 2_654 .
Co1 O2 H2A 123(2) . .
Co1 O2 H2B 109(3) . .
H2A O2 H2B 112(4) . .
O1 Co1 O1 82.71(7) . 2_654
O1 Co1 O2 84.55(7) . .
O1 Co1 O2 86.46(7) 2_654 .
O1 Co1 N2 173.14(7) . .
O1 Co1 N2 92.10(7) 2_654 .
O2 Co1 N2 90.68(8) . .
O1 Co1 N3 94.11(7) . .
O1 Co1 N3 176.49(7) 2_654 .
O2 Co1 N3 91.76(8) . .
N2 Co1 N3 90.95(7) . .
O1 Co1 N1 93.00(6) . .
O1 Co1 N1 91.33(6) 2_654 .
O2 Co1 N1 176.89(6) . .
N2 Co1 N1 91.59(7) . .
N3 Co1 N1 90.32(7) . .
O1 Co1 Co1 42.19(5) . 2_654
O1 Co1 Co1 41.96(5) 2_654 2_654
O2 Co1 Co1 92.58(5) . 2_654
N2 Co1 Co1 133.49(6) . 2_654
N3 Co1 Co1 135.23(6) . 2_654
N1 Co1 Co1 84.32(4) . 2_654
O5 N4 O4 122.40(18) . .
O5 N4 O3 118.49(18) . .
O4 N4 O3 119.11(17) . .
O7 N5 O6 129.9(3) . 5_655
O7 N5 O6 129.9(3) 5_655 .
O7 N5 O8 117.8(4) 5_655 .
O6 N5 O8 112.3(4) . .
O7 N5 O8 117.8(4) . 5_655
O6 N5 O8 112.3(4) 5_655 5_655
O7 O8 O6 102.8(4) . 5_655
O10 N6 O11 116.8(5) . 5_665
O10 N6 N6 116.8(5) . 5_665
O10 N6 O9 129.2(4) . .
O11 N6 O9 113.3(5) 5_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.338(2) .
C1 C2 1.401(3) .
C1 C6 1.532(3) .
C2 C3 1.358(3) .
C2 H2 0.9500 .
C3 C4 1.408(2) .
C3 H3 0.9500 .
C4 C3 1.408(2) 2_654
C4 C5 1.421(4) .
C5 N1 1.383(2) .
C5 N1 1.383(2) 2_654
C6 F1 1.382(2) .
C6 C7 1.510(3) .
C6 C12 1.516(3) .
C7 N2 1.341(3) .
C7 C8 1.380(3) .
C8 C9 1.390(3) .
C8 H8 0.9500 .
C9 C10 1.387(3) .
C9 H9 0.9500 .
C10 C11 1.378(3) .
C10 H10 0.9500 .
C11 N2 1.344(3) .
C11 H11 0.9500 .
C12 N3 1.345(3) .
C12 C13 1.379(3) .
C13 C14 1.390(3) .
C13 H13 0.9500 .
C14 C15 1.382(4) .
C14 H14 0.9500 .
C15 C16 1.387(3) .
C15 H15 0.9500 .
C16 N3 1.341(3) .
C16 H16 0.9500 .
N1 Co1 1.9408(16) .
N2 Co1 1.9182(19) .
N3 Co1 1.9306(19) .
O1 Co1 1.8703(16) .
O1 Co1 1.8787(17) 2_654
O1 H1A 0.73(3) .
O2 Co1 1.9077(14) .
O2 H2A 0.80(3) .
O2 H2B 0.89(4) .
Co1 O1 1.8787(17) 2_654
Co1 Co1 2.7826(5) 2_654
N4 O5 1.230(2) .
N4 O4 1.238(2) .
N4 O3 1.276(2) .
N5 O7 1.159(5) .
N5 O7 1.159(5) 5_655
N5 O6 1.232(5) 5_655
N5 O6 1.232(5) .
N5 O8 1.367(4) .
N5 O8 1.367(4) 5_655
N6 O10 1.016(4) .
N6 O11 1.248(5) 5_665
N6 O9 1.336(5) .
