# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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data_andr4

_chemical_name_systematic        
; 
 5,15-Diazatetrabenzo-10,20-bis(3,5-tert-butylphenyl)-porhyrin 
;
_chemical_name_common            ?
_chemical_melting_point_gt       623
_chemical_melting_point_lt       625
_chemical_formula_moiety         'C62 H60 N6'
_chemical_formula_sum            'C62 H60 N6'
_chemical_formula_weight         889.16

_exptl_crystal_description       Prism
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_preparation       Et₂O/CH₂Cl₂
_exptl_crystal_density_diffrn    1.061

_cell_length_a                   9.1332(15)
_cell_length_b                   11.8576(18)
_cell_length_c                   13.566(2)
_cell_angle_alpha                84.777(12)
_cell_angle_beta                 83.980(13)
_cell_angle_gamma                72.609(12)
_cell_volume                     1391.5(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_diffrn_ambient_temperature      295(2)

_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0537
_refine_ls_wR_factor_ref         0.1269
_refine_ls_wR_factor_gt          0.1146
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
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.6328(2) 0.44828(14) 1.11611(12) 0.0387(4) Uani 1 1 d . . .
H1 H 0.569(3) 0.479(2) 1.0692(18) 0.071(8) Uiso 1 1 d . . .
C2 C 0.7208(2) 0.33326(18) 1.12752(14) 0.0399(5) Uani 1 1 d . . .
C3 C 0.8188(2) 0.32021(17) 1.20819(14) 0.0389(5) Uani 1 1 d . . .
C4 C 0.9280(2) 0.22102(19) 1.24510(15) 0.0441(5) Uani 1 1 d . . .
H4 H 0.9497 0.1482 1.2176 0.053 Uiso 1 1 calc R . .
C5 C 1.0028(3) 0.23458(19) 1.32372(16) 0.0494(6) Uani 1 1 d . . .
H5 H 1.0772 0.1700 1.3500 0.059 Uiso 1 1 calc R . .
C6 C 0.9689(3) 0.3438(2) 1.36471(16) 0.0534(6) Uani 1 1 d . . .
H6 H 1.0208 0.3499 1.4185 0.064 Uiso 1 1 calc R . .
C7 C 0.8610(2) 0.44347(19) 1.32841(14) 0.0449(5) Uani 1 1 d . . .
H7 H 0.8409 0.5159 1.3563 0.054 Uiso 1 1 calc R . .
C8 C 0.7822(2) 0.43147(17) 1.24720(13) 0.0373(5) Uani 1 1 d . . .
C9 C 0.6679(2) 0.51221(16) 1.18588(13) 0.0345(4) Uani 1 1 d . . .
C10 C 0.3978(2) 0.36586(17) 0.80825(13) 0.0361(5) Uani 1 1 d . . .
C11 C 0.4983(2) 0.29262(17) 0.87190(13) 0.0373(5) Uani 1 1 d . . .
N12 N 0.5521(2) 0.33368(14) 0.95038(11) 0.0406(4) Uani 1 1 d . . .
C13 C 0.6463(3) 0.24187(17) 1.00090(14) 0.0415(5) Uani 1 1 d . . .
C14 C 0.6571(2) 0.13369(17) 0.95529(14) 0.0407(5) Uani 1 1 d . . .
C15 C 0.7371(3) 0.01683(18) 0.98167(16) 0.0580(7) Uani 1 1 d . . .
H15 H 0.7950 -0.0018 1.0365 0.070 Uiso 1 1 calc R . .
C16 C 0.7278(3) -0.0701(2) 0.92403(18) 0.0680(8) Uani 1 1 d . . .
H16 H 0.7825 -0.1487 0.9384 0.082 Uiso 1 1 calc R . .
C17 C 0.6365(3) -0.0404(2) 0.84424(18) 0.0650(7) Uani 1 1 d . . .
H17 H 0.6288 -0.1008 0.8076 0.078 Uiso 1 1 calc R . .
C18 C 0.5576(3) 0.07375(18) 0.81743(16) 0.0521(6) Uani 1 1 d . . .
H18 H 0.4999 0.0911 0.7625 0.063 Uiso 1 1 calc R . .
C19 C 0.5656(2) 0.16393(17) 0.87443(14) 0.0400(5) Uani 1 1 d . . .
N20 N 0.72628(9) 0.24083(6) 1.07775(5) 0.0436(4) Uani 1 1 d . . .
C21 C 0.34691(9) 0.31192(6) 0.72667(5) 0.0363(5) Uani 1 1 d R . .
C22 C 0.42824(9) 0.30274(6) 0.63377(5) 0.0389(5) Uani 1 1 d R . .
H22 H 0.5141 0.3303 0.6218 0.047 Uiso 1 1 calc R . .
C23 C 0.38124(9) 0.25236(6) 0.55876(5) 0.0379(5) Uani 1 1 d R . .
C24 C 0.25292(9) 0.21117(6) 0.57665(5) 0.0388(5) Uani 1 1 d R . .
H24 H 0.2215 0.1775 0.5265 0.047 Uiso 1 1 calc R . .
C25 C 0.17159(9) 0.22035(6) 0.66955(5) 0.0371(5) Uani 1 1 d R . .
C26 C 0.21859(9) 0.27073(6) 0.74456(5) 0.0385(5) Uani 1 1 d R . .
H26 H 0.1642 0.2769 0.8067 0.046 Uiso 1 1 calc R . .
C27 C 0.0218(3) 0.18235(19) 0.68834(15) 0.0457(5) Uani 1 1 d . . .
C28 C 0.0106(3) 0.0991(2) 0.61048(18) 0.0674(7) Uani 1 1 d . . .
H28A H -0.0901 0.0883 0.6179 0.101 Uiso 1 1 calc R . .
H28B H 0.0866 0.0238 0.6200 0.101 Uiso 1 1 calc R . .
H28C H 0.0285 0.1332 0.5451 0.101 Uiso 1 1 calc R . .
C29 C -0.1159(3) 0.2929(2) 0.6808(3) 0.0822(9) Uani 1 1 d . . .
H29A H -0.1037 0.3519 0.7207 0.123 Uiso 1 1 calc R . .
H29B H -0.2086 0.2731 0.7042 0.123 Uiso 1 1 calc R . .
H29C H -0.1220 0.3233 0.6129 0.123 Uiso 1 1 calc R . .
C30 C 0.0176(4) 0.1173(3) 0.78983(18) 0.0780(9) Uani 1 1 d . . .
H30A H 0.1169 0.0622 0.7994 0.117 Uiso 1 1 calc R . .
H30B H -0.0580 0.0753 0.7939 0.117 Uiso 1 1 calc R . .
H30C H -0.0087 0.1734 0.8403 0.117 Uiso 1 1 calc R . .
C31 C 0.4715(3) 0.2488(2) 0.45470(15) 0.0523(6) Uani 1 1 d . . .
C32 C 0.4335(4) 0.1705(4) 0.3877(2) 0.1295(17) Uani 1 1 d . . .
H32A H 0.4812 0.0892 0.4080 0.194 Uiso 1 1 calc R . .
H32B H 0.4710 0.1867 0.3207 0.194 Uiso 1 1 calc R . .
H32C H 0.3239 0.1853 0.3911 0.194 Uiso 1 1 calc R . .
C33 C 0.4302(5) 0.3760(3) 0.4071(2) 0.1264(15) Uani 1 1 d . . .
H33A H 0.3203 0.4081 0.4086 0.190 Uiso 1 1 calc R . .
H33B H 0.4737 0.3752 0.3395 0.190 Uiso 1 1 calc R . .
H33C H 0.4709 0.4239 0.4435 0.190 Uiso 1 1 calc R . .
C34 C 0.6420(3) 0.2127(4) 0.4644(2) 0.1262(16) Uani 1 1 d . . .
H34A H 0.6961 0.1970 0.4003 0.189 Uiso 1 1 calc R . .
H34B H 0.6701 0.1426 0.5081 0.189 Uiso 1 1 calc R . .
H34C H 0.6686 0.2755 0.4912 0.189 Uiso 1 1 calc R . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C2 1.365(3) . ?
N1 C9 1.383(2) . ?
N1 H1 0.88(2) . ?
C2 N20 1.3245(19) . ?
C2 C3 1.454(2) . ?
C3 C4 1.388(3) . ?
C3 C8 1.400(3) . ?
C4 C5 1.371(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.392(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.382(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.417(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.462(3) . ?
C9 C10 1.396(3) 2_667 ?
C10 C11 1.376(3) . ?
C10 C9 1.396(3) 2_667 ?
C10 C21 1.5049(17) . ?
C11 N12 1.400(2) . ?
C11 C19 1.463(3) . ?
N12 C13 1.350(2) . ?
C13 N20 1.3312(19) . ?
C13 C14 1.447(2) . ?
C14 C15 1.393(3) . ?
C14 C19 1.404(3) . ?
C15 C16 1.377(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.391(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.366(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.399(3) . ?
C18 H18 0.9300 . ?
C21 C26 1.3900 . ?
C21 C22 1.3900 . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 C24 1.3900 . ?
C23 C31 1.556(2) . ?
C24 C25 1.3900 . ?
C24 H24 0.9300 . ?
C25 C26 1.3900 . ?
C25 C27 1.554(2) . ?
C26 H26 0.9300 . ?
C27 C30 1.518(3) . ?
C27 C29 1.526(3) . ?
C27 C28 1.541(3) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.490(3) . ?
C31 C34 1.504(3) . ?
C31 C33 1.538(4) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?

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
_geom_angle_publ_flag
C2 N1 C9 108.54(16) . . ?
C2 N1 H1 126.7(16) . . ?
C9 N1 H1 124.6(16) . . ?
N20 C2 N1 129.89(16) . . ?
N20 C2 C3 120.48(17) . . ?
N1 C2 C3 109.62(16) . . ?
C4 C3 C8 123.35(17) . . ?
C4 C3 C2 130.10(18) . . ?
C8 C3 C2 106.55(17) . . ?
C5 C4 C3 117.39(19) . . ?
C5 C4 H4 121.3 . . ?
C3 C4 H4 121.3 . . ?
C4 C5 C6 120.8(2) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C7 C6 C5 122.41(18) . . ?
C7 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C6 C7 C8 117.70(19) . . ?
C6 C7 H7 121.1 . . ?
C8 C7 H7 121.1 . . ?
C3 C8 C7 118.30(18) . . ?
C3 C8 C9 106.51(15) . . ?
C7 C8 C9 135.12(18) . . ?
N1 C9 C10 123.11(16) . 2_667 ?
N1 C9 C8 108.68(16) . . ?
C10 C9 C8 128.21(15) 2_667 . ?
C11 C10 C9 125.81(15) . 2_667 ?
C11 C10 C21 118.64(15) . . ?
C9 C10 C21 115.50(14) 2_667 . ?
C10 C11 N12 123.17(17) . . ?
C10 C11 C19 129.36(15) . . ?
N12 C11 C19 107.46(16) . . ?
C13 N12 C11 109.92(16) . . ?
N20 C13 N12 130.11(16) . . ?
N20 C13 C14 121.12(17) . . ?
N12 C13 C14 108.73(15) . . ?
C15 C14 C19 122.16(17) . . ?
C15 C14 C13 130.12(18) . . ?
C19 C14 C13 107.71(17) . . ?
C16 C15 C14 117.9(2) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
C15 C16 C17 120.0(2) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C18 C17 C16 122.7(2) . . ?
C18 C17 H17 118.7 . . ?
C16 C17 H17 118.7 . . ?
C17 C18 C19 118.51(19) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
C18 C19 C14 118.69(18) . . ?
C18 C19 C11 135.14(18) . . ?
C14 C19 C11 106.17(15) . . ?
C2 N20 C13 126.25(13) . . ?
C26 C21 C22 120.0 . . ?
C26 C21 C10 119.82(8) . . ?
C22 C21 C10 120.18(8) . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C24 C23 C22 120.0 . . ?
C24 C23 C31 121.72(8) . . ?
C22 C23 C31 118.23(8) . . ?
C23 C24 C25 120.0 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C26 C25 C24 120.0 . . ?
C26 C25 C27 119.44(8) . . ?
C24 C25 C27 120.44(8) . . ?
C21 C26 C25 120.0 . . ?
C21 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C30 C27 C29 111.2(3) . . ?
C30 C27 C28 107.79(19) . . ?
C29 C27 C28 107.42(19) . . ?
C30 C27 C25 109.77(16) . . ?
C29 C27 C25 108.51(17) . . ?
C28 C27 C25 112.13(17) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C34 110.4(3) . . ?
C32 C31 C33 108.9(3) . . ?
C34 C31 C33 105.9(3) . . ?
C32 C31 C23 113.09(19) . . ?
C34 C31 C23 110.66(18) . . ?
C33 C31 C23 107.6(2) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 C2 N20 180.0(2) . . . . ?
C9 N1 C2 C3 -0.1(2) . . . . ?
N20 C2 C3 C4 1.2(3) . . . . ?
N1 C2 C3 C4 -178.8(2) . . . . ?
N20 C2 C3 C8 -178.04(18) . . . . ?
N1 C2 C3 C8 2.0(2) . . . . ?
C8 C3 C4 C5 -0.1(3) . . . . ?
C2 C3 C4 C5 -179.2(2) . . . . ?
C3 C4 C5 C6 0.4(3) . . . . ?
C4 C5 C6 C7 -0.7(4) . . . . ?
C5 C6 C7 C8 0.8(3) . . . . ?
C4 C3 C8 C7 0.1(3) . . . . ?
C2 C3 C8 C7 179.42(19) . . . . ?
C4 C3 C8 C9 177.7(2) . . . . ?
C2 C3 C8 C9 -3.0(2) . . . . ?
C6 C7 C8 C3 -0.5(3) . . . . ?
C6 C7 C8 C9 -177.2(2) . . . . ?
C2 N1 C9 C10 177.4(2) . . . 2_667 ?
C2 N1 C9 C8 -1.8(2) . . . . ?
C3 C8 C9 N1 3.0(2) . . . . ?
C7 C8 C9 N1 -180.0(2) . . . . ?
C3 C8 C9 C10 -176.1(2) . . . 2_667 ?
C7 C8 C9 C10 0.9(4) . . . 2_667 ?
C9 C10 C11 N12 -2.3(3) 2_667 . . . ?
C21 C10 C11 N12 -179.69(17) . . . . ?
C9 C10 C11 C19 176.3(2) 2_667 . . . ?
C21 C10 C11 C19 -1.0(3) . . . . ?
C10 C11 N12 C13 178.89(19) . . . . ?
C19 C11 N12 C13 0.0(2) . . . . ?
C11 N12 C13 N20 177.4(2) . . . . ?
C11 N12 C13 C14 -0.2(2) . . . . ?
N20 C13 C14 C15 3.7(4) . . . . ?
N12 C13 C14 C15 -178.5(2) . . . . ?
N20 C13 C14 C19 -177.50(18) . . . . ?
N12 C13 C14 C19 0.3(2) . . . . ?
C19 C14 C15 C16 1.7(4) . . . . ?
C13 C14 C15 C16 -179.6(2) . . . . ?
C14 C15 C16 C17 -2.1(4) . . . . ?
C15 C16 C17 C18 2.3(4) . . . . ?
C16 C17 C18 C19 -1.9(4) . . . . ?
C17 C18 C19 C14 1.4(3) . . . . ?
C17 C18 C19 C11 -178.6(2) . . . . ?
C15 C14 C19 C18 -1.4(3) . . . . ?
C13 C14 C19 C18 179.7(2) . . . . ?
C15 C14 C19 C11 178.6(2) . . . . ?
C13 C14 C19 C11 -0.3(2) . . . . ?
C10 C11 C19 C18 1.4(4) . . . . ?
N12 C11 C19 C18 -179.7(3) . . . . ?
C10 C11 C19 C14 -178.6(2) . . . . ?
N12 C11 C19 C14 0.2(2) . . . . ?
N1 C2 N20 C13 2.1(3) . . . . ?
C3 C2 N20 C13 -177.85(18) . . . . ?
N12 C13 N20 C2 5.6(3) . . . . ?
C14 C13 N20 C2 -177.16(19) . . . . ?
C11 C10 C21 C26 88.25(17) . . . . ?
C9 C10 C21 C26 -89.38(16) 2_667 . . . ?
C11 C10 C21 C22 -91.45(16) . . . . ?
C9 C10 C21 C22 90.92(17) 2_667 . . . ?
C26 C21 C22 C23 0.0 . . . . ?
C10 C21 C22 C23 179.70(9) . . . . ?
C21 C22 C23 C24 0.0 . . . . ?
C21 C22 C23 C31 177.44(11) . . . . ?
C22 C23 C24 C25 0.0 . . . . ?
C31 C23 C24 C25 -177.35(12) . . . . ?
C23 C24 C25 C26 0.0 . . . . ?
C23 C24 C25 C27 175.91(10) . . . . ?
C22 C21 C26 C25 0.0 . . . . ?
C10 C21 C26 C25 -179.70(9) . . . . ?
C24 C25 C26 C21 0.0 . . . . ?
C27 C25 C26 C21 -175.95(10) . . . . ?
C26 C25 C27 C30 -44.6(2) . . . . ?
C24 C25 C27 C30 139.43(16) . . . . ?
C26 C25 C27 C29 77.09(18) . . . . ?
C24 C25 C27 C29 -98.84(18) . . . . ?
C26 C25 C27 C28 -164.42(13) . . . . ?
C24 C25 C27 C28 19.6(2) . . . . ?
C24 C23 C31 C32 -15.1(3) . . . . ?
C22 C23 C31 C32 167.5(2) . . . . ?
C24 C23 C31 C34 -139.6(2) . . . . ?
C22 C23 C31 C34 43.0(3) . . . . ?
C24 C23 C31 C33 105.2(2) . . . . ?
C22 C23 C31 C33 -72.2(2) . . . . ?

############################################################################ 

_audit_creation_method           SHELXL97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_cell_measurement_reflns_used    8367
_cell_measurement_theta_min      3.92
_cell_measurement_theta_max      70.10

_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             474
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_factor_muR        0.024
_exptl_absorpt_process_details   
;
 Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_absorpt_correction_T_min  0.2901
_exptl_absorpt_correction_T_max  1.0000
_exptl_special_details           ?

_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_measurement_method       'rotation method'
_diffrn_measurement_details      '3493 frames, detector distance = 60 mm'
_diffrn_measurement_device_type  'Stoe STADI VARI'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4785
_diffrn_reflns_av_R_equivalents  
0.0 #Rint=0.0271 before absorption correction 
_diffrn_reflns_av_sigmaI/netI    0.0981
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.91
_diffrn_reflns_theta_max         70.09
_reflns_number_total             4785
_reflns_number_gt                2788
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'X--AREA  (STOE & CIE, 2012)'
_computing_cell_refinement       'X--AREA  (STOE & CIE, 2012)'
_computing_data_reduction        'X--RED   (STOE & CIE, 2012)'
_computing_structure_solution    'SHELXS97 (Sheldrick,  2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick,  2008)'
_computing_molecular_graphics    'Ortep--3 (Farrugia,   1997)'
_computing_publication_material  'WinGX    (Farrugia,   1999)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0653P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4785
_refine_ls_number_parameters     299
_refine_ls_number_restraints     0
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_restrained_S_all      0.864
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_geom_special_details            
; 
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix. The cell s.u.'s are taken 
 into account individually in the estimation of s.u.'s in distances, angles 
 and torsion angles; correlations between s.u.'s in cell parameters are only 
 used when they are defined by crystal symmetry. An approximate (isotropic) 
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. 
;

_diffrn_measured_fraction_theta_max 0.907
_diffrn_reflns_theta_full        70.09
_diffrn_measured_fraction_theta_full 0.907
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.051
#########################################################

_database_code_depnum_ccdc_archive 'CCDC 989911'
