#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/68/1516868.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_1516868
loop_
_publ_author_name
'Ryoji Mitsuhashi'
'Takayoshi Suzuki'
'Yukinari Sunatsuki'
'Masaaki Kojima'
_publ_section_title
;
 Hydrogen-bonding interactions, geometrical selectivity and spectroscopic
 properties of cobalt(III) complexes with unsymmetrical tridentate
 amine-amidato-phenolato type ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              131
_journal_page_last               137
_journal_volume                  399
_journal_year                    2013
_chemical_formula_moiety
'P C24 H20 1+, C22 H28 Co N4 O4 1-, 1.5(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C49 H56.5 Co N5.5 O6 P'
_chemical_formula_weight         908.40
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.372(3)
_cell_angle_beta                 96.621(3)
_cell_angle_gamma                112.716(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5973(11)
_cell_length_b                   12.2755(11)
_cell_length_c                   18.0998(15)
_cell_measurement_reflns_used    15457
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2289.0(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'CrystalStructure 3.8'
_computing_molecular_graphics    'ortep-3 for win'
_computing_publication_material  SHELXL97
_computing_structure_refinement  SHELXL97
_computing_structure_solution    'DIRDIF99 (PATTY)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20579
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.8731
_exptl_absorpt_correction_T_min  0.8008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             958
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         10368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1105P)²+1.1399P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1669
_reflns_number_gt                9016
_reflns_number_total             10368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-399-131-137-2.cif
_cod_data_source_block           PPh4[1]_1.5CH3CN_2H2O
_cod_original_formula_sum        'C49 H56.50 Co N5.50 O6 P'
_cod_database_code               1516868
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
Co1 Co 0.34399(2) 0.06706(3) 0.357987(14) 0.02226(11) Uani 1 1 d .
P1 P 0.22520(5) 0.31538(5) 0.00360(3) 0.02206(13) Uani 1 1 d .
O1 O 0.40793(15) 0.21458(15) 0.32707(9) 0.0308(3) Uani 1 1 d .
O2 O 0.02138(15) 0.02324(15) 0.21342(10) 0.0324(4) Uani 1 1 d .
O3 O 0.39071(15) -0.01104(16) 0.27419(9) 0.0309(3) Uani 1 1 d .
O4 O 0.70333(16) 0.1297(2) 0.46717(10) 0.0428(5) Uani 1 1 d .
O5 O 0.6574(12) 0.3728(11) 0.3222(8) 0.159(4) Uiso 0.50 1 d P
O6 O 0.755(2) 0.393(2) 0.3836(14) 0.265(9) Uiso 0.50 1 d P
O7 O 0.8493(16) 0.5152(17) 0.4305(10) 0.197(6) Uiso 0.50 1 d P
O8 O 0.0728(12) 0.3236(12) 0.4505(7) 0.168(4) Uiso 0.50 1 d P
N1 N 0.17912(16) 0.01077(17) 0.29441(10) 0.0243(4) Uani 1 1 d .
N2 N 0.27350(17) -0.09257(17) 0.38260(10) 0.0269(4) Uani 1 1 d .
H2A H 0.3174 -0.1368 0.3648 0.032 Uiso 1 1 calc R
H2B H 0.2854 -0.0812 0.4350 0.032 Uiso 1 1 calc R
N3 N 0.50287(17) 0.11541(18) 0.42774(10) 0.0281(4) Uani 1 1 d .
N4 N 0.29661(18) 0.14455(17) 0.44630(10) 0.0274(4) Uani 1 1 d .
H4A H 0.2608 0.1942 0.4313 0.033 Uiso 1 1 calc R
H4B H 0.2357 0.0853 0.4628 0.033 Uiso 1 1 calc R
N5 N 0.800(2) 0.365(2) 0.2947(13) 0.195(9) Uiso 0.50 1 d P
N6 N 0.2251(13) 0.4584(13) 0.5902(8) 0.135(4) Uiso 0.50 1 d P
N7 N 0.8491(11) 0.3601(11) 0.0843(8) 0.127(4) Uiso 0.50 1 d P
C1 C 0.3346(2) 0.2682(2) 0.30718(12) 0.0300(5) Uani 1 1 d .
C2 C 0.3943(3) 0.3942(2) 0.31342(14) 0.0426(6) Uani 1 1 d .
H2 H 0.4837 0.4367 0.3327 0.051 Uiso 1 1 calc R
C3 C 0.3247(3) 0.4579(2) 0.29181(16) 0.0504(8) Uani 1 1 d .
H3 H 0.3671 0.5430 0.2965 0.060 Uiso 1 1 calc R
C4 C 0.1949(3) 0.3987(3) 0.26379(16) 0.0491(7) Uani 1 1 d .
H4 H 0.1475 0.4427 0.2500 0.059 Uiso 1 1 calc R
C5 C 0.1344(3) 0.2742(2) 0.25603(14) 0.0371(5) Uani 1 1 d .
H5 H 0.0451 0.2334 0.2360 0.044 Uiso 1 1 calc R
C6 C 0.2007(2) 0.2068(2) 0.27678(12) 0.0275(4) Uani 1 1 d .
C7 C 0.1271(2) 0.0719(2) 0.25922(11) 0.0242(4) Uani 1 1 d .
C8 C 0.1131(2) -0.1216(2) 0.27541(12) 0.0267(4) Uani 1 1 d .
H8A H 0.1476 -0.1577 0.2350 0.032 Uiso 1 1 calc R
H8B H 0.0208 -0.1475 0.2561 0.032 Uiso 1 1 calc R
C9 C 0.1336(2) -0.1639(2) 0.34804(13) 0.0300(5) Uani 1 1 d .
C10 C 0.0558(2) -0.1329(3) 0.40442(14) 0.0371(5) Uani 1 1 d .
H10A H 0.0778 -0.0453 0.4154 0.045 Uiso 1 1 calc R
H10B H 0.0751 -0.1552 0.4521 0.045 Uiso 1 1 calc R
H10C H -0.0355 -0.1782 0.3818 0.045 Uiso 1 1 calc R
C11 C 0.0996(3) -0.2993(2) 0.33053(17) 0.0435(6) Uani 1 1 d .
H11A H 0.1141 -0.3230 0.3785 0.052 Uiso 1 1 calc R
H11B H 0.1533 -0.3180 0.2968 0.052 Uiso 1 1 calc R
H11C H 0.0096 -0.3444 0.3050 0.052 Uiso 1 1 calc R
C12 C 0.5101(2) 0.01098(19) 0.27019(12) 0.0250(4) Uani 1 1 d .
C13 C 0.5338(2) -0.0219(2) 0.19628(13) 0.0278(4) Uani 1 1 d .
H13 H 0.4654 -0.0531 0.1530 0.033 Uiso 1 1 calc R
C14 C 0.6533(2) -0.0098(2) 0.18538(14) 0.0329(5) Uani 1 1 d .
H14 H 0.6665 -0.0318 0.1350 0.039 Uiso 1 1 calc R
C15 C 0.7552(2) 0.0346(2) 0.24791(16) 0.0353(5) Uani 1 1 d .
H15 H 0.8373 0.0412 0.2408 0.042 Uiso 1 1 calc R
C16 C 0.7342(2) 0.0686(2) 0.32013(14) 0.0321(5) Uani 1 1 d .
H16 H 0.8036 0.0990 0.3627 0.039 Uiso 1 1 calc R
C17 C 0.6150(2) 0.0602(2) 0.33321(13) 0.0273(4) Uani 1 1 d .
C18 C 0.6073(2) 0.1042(2) 0.41447(13) 0.0301(5) Uani 1 1 d .
C19 C 0.4982(2) 0.1566(2) 0.50781(12) 0.0318(5) Uani 1 1 d .
H19A H 0.5848 0.2141 0.5369 0.038 Uiso 1 1 calc R
H19B H 0.4683 0.0861 0.5310 0.038 Uiso 1 1 calc R
C20 C 0.4082(2) 0.2191(2) 0.51224(12) 0.0296(5) Uani 1 1 d .
C21 C 0.3621(3) 0.2197(3) 0.58793(14) 0.0407(6) Uani 1 1 d .
H21A H 0.3224 0.1360 0.5935 0.049 Uiso 1 1 calc R
H21B H 0.2995 0.2550 0.5882 0.049 Uiso 1 1 calc R
H21C H 0.4349 0.2683 0.6306 0.049 Uiso 1 1 calc R
C22 C 0.4700(3) 0.3475(2) 0.50201(15) 0.0406(6) Uani 1 1 d .
H22A H 0.4095 0.3852 0.5051 0.049 Uiso 1 1 calc R
H22B H 0.4942 0.3449 0.4518 0.049 Uiso 1 1 calc R
H22C H 0.5464 0.3954 0.5425 0.049 Uiso 1 1 calc R
C23 C 0.2483(2) 0.45577(19) 0.06700(12) 0.0258(4) Uani 1 1 d .
C24 C 0.3697(2) 0.5374(2) 0.10809(13) 0.0295(4) Uani 1 1 d .
H24 H 0.4401 0.5164 0.1055 0.035 Uiso 1 1 calc R
C25 C 0.3877(2) 0.6493(2) 0.15282(14) 0.0340(5) Uani 1 1 d .
H25 H 0.4707 0.7054 0.1803 0.041 Uiso 1 1 calc R
C26 C 0.2851(3) 0.6792(2) 0.15738(15) 0.0387(5) Uani 1 1 d .
H26 H 0.2975 0.7561 0.1877 0.046 Uiso 1 1 calc R
C27 C 0.1636(3) 0.5966(3) 0.11753(18) 0.0453(6) Uani 1 1 d .
H27 H 0.0930 0.6168 0.1215 0.054 Uiso 1 1 calc R
C28 C 0.1444(2) 0.4851(2) 0.07217(15) 0.0375(5) Uani 1 1 d .
H28 H 0.0613 0.4292 0.0448 0.045 Uiso 1 1 calc R
C29 C 0.3445(2) 0.26825(18) 0.04016(12) 0.0241(4) Uani 1 1 d .
C30 C 0.3548(2) 0.2509(2) 0.11496(13) 0.0292(4) Uani 1 1 d .
H30 H 0.3017 0.2679 0.1472 0.035 Uiso 1 1 calc R
C31 C 0.4430(2) 0.2089(2) 0.14137(13) 0.0330(5) Uani 1 1 d .
H31 H 0.4481 0.1943 0.1912 0.040 Uiso 1 1 calc R
C32 C 0.5236(2) 0.1883(2) 0.09543(14) 0.0330(5) Uani 1 1 d .
H32 H 0.5835 0.1591 0.1137 0.040 Uiso 1 1 calc R
C33 C 0.5173(2) 0.2100(2) 0.02287(14) 0.0312(5) Uani 1 1 d .
H33 H 0.5751 0.1987 -0.0076 0.037 Uiso 1 1 calc R
C34 C 0.4268(2) 0.2481(2) -0.00547(12) 0.0269(4) Uani 1 1 d .
H34 H 0.4209 0.2604 -0.0559 0.032 Uiso 1 1 calc R
C35 C 0.0654(2) 0.20549(19) -0.00379(12) 0.0254(4) Uani 1 1 d .
C36 C 0.0325(2) 0.1562(2) 0.05838(14) 0.0355(5) Uani 1 1 d .
H36 H 0.0961 0.1738 0.1023 0.043 Uiso 1 1 calc R
C37 C -0.0937(3) 0.0813(2) 0.05544(15) 0.0395(6) Uani 1 1 d .
H37 H -0.1168 0.0478 0.0977 0.047 Uiso 1 1 calc R
C38 C -0.1866(2) 0.0548(2) -0.00870(15) 0.0354(5) Uani 1 1 d .
H38 H -0.2734 0.0057 -0.0094 0.043 Uiso 1 1 calc R
C39 C -0.1537(2) 0.0995(2) -0.07168(15) 0.0353(5) Uani 1 1 d .
H39 H -0.2170 0.0784 -0.1164 0.042 Uiso 1 1 calc R
C40 C -0.0275(2) 0.1754(2) -0.06924(13) 0.0311(5) Uani 1 1 d .
H40 H -0.0045 0.2068 -0.1123 0.037 Uiso 1 1 calc R
C41 C 0.24698(19) 0.34022(19) -0.08949(12) 0.0236(4) Uani 1 1 d .
C42 C 0.2220(2) 0.2412(2) -0.15059(12) 0.0262(4) Uani 1 1 d .
H42 H 0.1888 0.1608 -0.1435 0.031 Uiso 1 1 calc R
C43 C 0.2457(2) 0.2605(2) -0.22166(13) 0.0306(5) Uani 1 1 d .
H43 H 0.2299 0.1937 -0.2632 0.037 Uiso 1 1 calc R
C44 C 0.2927(2) 0.3787(2) -0.23161(14) 0.0368(5) Uani 1 1 d .
H44 H 0.3090 0.3923 -0.2802 0.044 Uiso 1 1 calc R
C45 C 0.3157(3) 0.4751(2) -0.17195(15) 0.0386(6) Uani 1 1 d .
H45 H 0.3473 0.5552 -0.1796 0.046 Uiso 1 1 calc R
C46 C 0.2933(2) 0.4577(2) -0.10020(13) 0.0313(5) Uani 1 1 d .
H46 H 0.3095 0.5252 -0.0590 0.038 Uiso 1 1 calc R
C47 C 0.8256(13) 0.3492(13) 0.2642(10) 0.097(3) Uiso 0.50 1 d P
C48 C 0.8577(10) 0.3557(10) 0.1730(9) 0.084(3) Uiso 0.50 1 d P
C49 C 0.1774(17) 0.4578(17) 0.5181(12) 0.143(5) Uiso 0.50 1 d P
C50 C 0.1624(15) 0.5251(16) 0.4740(10) 0.137(5) Uiso 0.50 1 d P
C51 C 0.8594(8) 0.3536(7) 0.1316(6) 0.0622(18) Uiso 0.50 1 d P
C52 C 0.8498(11) 0.3434(10) 0.2164(9) 0.087(3) Uiso 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'
O O 0.0106 0.0060 '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'
P P 0.1023 0.0942 '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
O1 Co1 O3 90.44(8) . .
O1 Co1 N1 93.34(7) . .
O3 Co1 N1 87.48(7) . .
O1 Co1 N3 91.02(8) . .
O3 Co1 N3 94.80(7) . .
N1 Co1 N3 175.07(8) . .
O1 Co1 N4 91.01(8) . .
O3 Co1 N4 178.31(8) . .
N1 Co1 N4 93.30(8) . .
N3 Co1 N4 84.30(8) . .
O1 Co1 N2 176.02(7) . .
O3 Co1 N2 86.33(8) . .
N1 Co1 N2 84.21(8) . .
N3 Co1 N2 91.56(8) . .
N4 Co1 N2 92.26(8) . .
C35 P1 C23 108.70(10) . .
C35 P1 C41 109.27(10) . .
C23 P1 C41 109.25(10) . .
C35 P1 C29 112.90(10) . .
C23 P1 C29 108.39(10) . .
C41 P1 C29 108.27(10) . .
C1 O1 Co1 122.30(14) . .
C12 O3 Co1 123.19(14) . .
O6 O5 N5 65.0(11) . .
O5 O6 O7 125.4(19) . .
O5 O6 N6 88.8(14) . 2_666
O7 O6 N6 38.8(9) . 2_666
C49 O7 N6 78.7(18) 2_666 2_666
C49 O7 O6 113(2) 2_666 .
N6 O7 O6 81.8(16) 2_666 .
C49 O7 C50 41.0(13) 2_666 2_666
N6 O7 C50 113.3(16) 2_666 2_666
O6 O7 C50 95.6(14) . 2_666
C7 N1 C8 118.19(17) . .
C7 N1 Co1 129.61(15) . .
C8 N1 Co1 111.56(13) . .
C9 N2 Co1 112.54(13) . .
C9 N2 H2A 109.1 . .
Co1 N2 H2A 109.1 . .
C9 N2 H2B 109.1 . .
Co1 N2 H2B 109.1 . .
H2A N2 H2B 107.8 . .
C18 N3 C19 116.89(18) . .
C18 N3 Co1 129.28(16) . .
C19 N3 Co1 113.38(15) . .
C20 N4 Co1 113.09(14) . .
C20 N4 H4A 109.0 . .
Co1 N4 H4A 109.0 . .
C20 N4 H4B 109.0 . .
Co1 N4 H4B 109.0 . .
H4A N4 H4B 107.8 . .
C47 N5 O5 144(3) . .
O7 N6 C49 49.5(12) 2_666 .
O7 N6 O6 59.4(12) 2_666 2_666
C49 N6 O6 87.0(14) . 2_666
O1 C1 C2 117.2(2) . .
O1 C1 C6 124.7(2) . .
C2 C1 C6 118.1(2) . .
C3 C2 C1 121.1(3) . .
C3 C2 H2 119.4 . .
C1 C2 H2 119.4 . .
C4 C3 C2 120.7(3) . .
C4 C3 H3 119.7 . .
C2 C3 H3 119.7 . .
C3 C4 C5 119.1(3) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C4 C5 C6 122.0(3) . .
C4 C5 H5 119.0 . .
C6 C5 H5 119.0 . .
C5 C6 C1 118.9(2) . .
C5 C6 C7 116.8(2) . .
C1 C6 C7 124.0(2) . .
O2 C7 N1 124.0(2) . .
O2 C7 C6 119.16(19) . .
N1 C7 C6 116.79(18) . .
N1 C8 C9 107.94(17) . .
N1 C8 H8A 110.1 . .
C9 C8 H8A 110.1 . .
N1 C8 H8B 110.1 . .
C9 C8 H8B 110.1 . .
H8A C8 H8B 108.4 . .
N2 C9 C11 110.4(2) . .
N2 C9 C8 104.80(17) . .
C11 C9 C8 111.9(2) . .
N2 C9 C10 109.16(19) . .
C11 C9 C10 109.8(2) . .
C8 C9 C10 110.8(2) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C9 C11 H11A 109.5 . .
C9 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C9 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
O3 C12 C13 116.44(19) . .
O3 C12 C17 125.9(2) . .
C13 C12 C17 117.6(2) . .
C14 C13 C12 121.7(2) . .
C14 C13 H13 119.1 . .
C12 C13 H13 119.1 . .
C13 C14 C15 120.4(2) . .
C13 C14 H14 119.8 . .
C15 C14 H14 119.8 . .
C16 C15 C14 118.6(2) . .
C16 C15 H15 120.7 . .
C14 C15 H15 120.7 . .
C15 C16 C17 122.6(2) . .
C15 C16 H16 118.7 . .
C17 C16 H16 118.7 . .
C16 C17 C12 118.9(2) . .
C16 C17 C18 116.7(2) . .
C12 C17 C18 124.33(19) . .
O4 C18 N3 123.5(2) . .
O4 C18 C17 118.0(2) . .
N3 C18 C17 118.54(19) . .
N3 C19 C20 109.73(18) . .
N3 C19 H19A 109.7 . .
C20 C19 H19A 109.7 . .
N3 C19 H19B 109.7 . .
C20 C19 H19B 109.7 . .
H19A C19 H19B 108.2 . .
N4 C20 C22 108.61(19) . .
N4 C20 C19 105.59(18) . .
C22 C20 C19 111.5(2) . .
N4 C20 C21 109.74(19) . .
C22 C20 C21 110.6(2) . .
C19 C20 C21 110.6(2) . .
C20 C21 H21A 109.5 . .
C20 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C20 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C20 C22 H22A 109.5 . .
C20 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C20 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C28 C23 C24 120.1(2) . .
C28 C23 P1 119.33(17) . .
C24 C23 P1 120.52(17) . .
C25 C24 C23 120.0(2) . .
C25 C24 H24 120.0 . .
C23 C24 H24 120.0 . .
C26 C25 C24 120.0(2) . .
C26 C25 H25 120.0 . .
C24 C25 H25 120.0 . .
C25 C26 C27 119.9(2) . .
C25 C26 H26 120.1 . .
C27 C26 H26 120.1 . .
C28 C27 C26 120.7(2) . .
C28 C27 H27 119.6 . .
C26 C27 H27 119.6 . .
C27 C28 C23 119.3(2) . .
C27 C28 H28 120.3 . .
C23 C28 H28 120.3 . .
C34 C29 C30 119.6(2) . .
C34 C29 P1 120.31(16) . .
C30 C29 P1 120.08(17) . .
C31 C30 C29 119.7(2) . .
C31 C30 H30 120.2 . .
C29 C30 H30 120.2 . .
C32 C31 C30 120.2(2) . .
C32 C31 H31 119.9 . .
C30 C31 H31 119.9 . .
C31 C32 C33 120.3(2) . .
C31 C32 H32 119.9 . .
C33 C32 H32 119.9 . .
C32 C33 C34 120.2(2) . .
C32 C33 H33 119.9 . .
C34 C33 H33 119.9 . .
C33 C34 C29 119.9(2) . .
C33 C34 H34 120.1 . .
C29 C34 H34 120.1 . .
C40 C35 C36 120.0(2) . .
C40 C35 P1 120.31(17) . .
C36 C35 P1 119.58(17) . .
C37 C36 C35 119.3(2) . .
C37 C36 H36 120.3 . .
C35 C36 H36 120.3 . .
C36 C37 C38 120.5(2) . .
C36 C37 H37 119.7 . .
C38 C37 H37 119.7 . .
C39 C38 C37 120.3(2) . .
C39 C38 H38 119.8 . .
C37 C38 H38 119.8 . .
C38 C39 C40 119.6(2) . .
C38 C39 H39 120.2 . .
C40 C39 H39 120.2 . .
C39 C40 C35 120.1(2) . .
C39 C40 H40 120.0 . .
C35 C40 H40 120.0 . .
C46 C41 C42 120.1(2) . .
C46 C41 P1 120.25(17) . .
C42 C41 P1 119.62(16) . .
C43 C42 C41 119.9(2) . .
C43 C42 H42 120.0 . .
C41 C42 H42 120.0 . .
C42 C43 C44 119.5(2) . .
C42 C43 H43 120.2 . .
C44 C43 H43 120.2 . .
C45 C44 C43 120.4(2) . .
C45 C44 H44 119.8 . .
C43 C44 H44 119.8 . .
C44 C45 C46 121.0(2) . .
C44 C45 H45 119.5 . .
C46 C45 H45 119.5 . .
C41 C46 C45 119.1(2) . .
C41 C46 H46 120.4 . .
C45 C46 H46 120.4 . .
N5 C47 C48 151(3) . .
O7 C49 C50 107(2) 2_666 .
O7 C49 N6 51.8(13) 2_666 .
C50 C49 N6 144.5(19) . .
C49 C50 O7 32.2(11) . 2_666
N7 C51 C52 167.8(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 1.8883(17) .
Co1 O3 1.8921(16) .
Co1 N1 1.9088(17) .
Co1 N3 1.9211(18) .
Co1 N4 1.9546(19) .
Co1 N2 1.9666(19) .
P1 C35 1.794(2) .
P1 C23 1.794(2) .
P1 C41 1.794(2) .
P1 C29 1.797(2) .
O1 C1 1.317(3) .
O2 C7 1.252(3) .
O3 C12 1.318(3) .
O4 C18 1.275(3) .
O5 O6 1.40(2) .
O5 N5 1.82(2) .
O6 O7 1.49(2) .
O6 N6 1.71(3) 2_666
O7 C49 1.05(2) 2_666
O7 N6 1.085(17) 2_666
O7 C50 1.89(2) 2_666
N1 C7 1.329(3) .
N1 C8 1.457(3) .
N2 C9 1.504(3) .
N2 H2A 0.9200 .
N2 H2B 0.9200 .
N3 C18 1.314(3) .
N3 C19 1.461(3) .
N4 C20 1.507(3) .
N4 H4A 0.9200 .
N4 H4B 0.9200 .
N5 C47 0.69(2) .
N6 O7 1.085(17) 2_666
N6 C49 1.35(2) .
N6 O6 1.71(3) 2_666
N7 C51 0.874(13) .
C1 C2 1.406(3) .
C1 C6 1.425(3) .
C2 C3 1.393(4) .
C2 H2 0.9500 .
C3 C4 1.377(5) .
C3 H3 0.9500 .
C4 C5 1.386(4) .
C4 H4 0.9500 .
C5 C6 1.398(3) .
C5 H5 0.9500 .
C6 C7 1.493(3) .
C8 C9 1.525(3) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C11 1.514(3) .
C9 C10 1.529(3) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 C13 1.415(3) .
C12 C17 1.418(3) .
C13 C14 1.378(3) .
C13 H13 0.9500 .
C14 C15 1.395(4) .
C14 H14 0.9500 .
C15 C16 1.377(4) .
C15 H15 0.9500 .
C16 C17 1.398(3) .
C16 H16 0.9500 .
C17 C18 1.498(3) .
C19 C20 1.517(3) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 C22 1.515(3) .
C20 C21 1.527(3) .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 C28 1.392(3) .
C23 C24 1.393(3) .
C24 C25 1.388(3) .
C24 H24 0.9500 .
C25 C26 1.381(4) .
C25 H25 0.9500 .
C26 C27 1.391(4) .
C26 H26 0.9500 .
C27 C28 1.383(4) .
C27 H27 0.9500 .
C28 H28 0.9500 .
C29 C34 1.395(3) .
C29 C30 1.407(3) .
C30 C31 1.386(3) .
C30 H30 0.9500 .
C31 C32 1.384(4) .
C31 H31 0.9500 .
C32 C33 1.386(3) .
C32 H32 0.9500 .
C33 C34 1.387(3) .
C33 H33 0.9500 .
C34 H34 0.9500 .
C35 C40 1.394(3) .
C35 C36 1.394(3) .
C36 C37 1.384(3) .
C36 H36 0.9500 .
C37 C38 1.385(4) .
C37 H37 0.9500 .
C38 C39 1.382(4) .
C38 H38 0.9500 .
C39 C40 1.388(3) .
C39 H39 0.9500 .
C40 H40 0.9500 .
C41 C46 1.390(3) .
C41 C42 1.398(3) .
C42 C43 1.388(3) .
C42 H42 0.9500 .
C43 C44 1.392(3) .
C43 H43 0.9500 .
C44 C45 1.367(4) .
C44 H44 0.9500 .
C45 C46 1.391(3) .
C45 H45 0.9500 .
C46 H46 0.9500 .
C47 C48 1.741(19) .
C49 O7 1.05(2) 2_666
C49 C50 1.29(2) .
C50 O7 1.89(2) 2_666
C51 C52 1.575(15) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2B O4 0.920 1.972 2.836(2) 155.77 2_656
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_4
O3 Co1 O1 C1 118.26(16) . .
N1 Co1 O1 C1 30.76(17) . .
N3 Co1 O1 C1 -146.93(17) . .
N4 Co1 O1 C1 -62.61(17) . .
N2 Co1 O1 C1 82.6(11) . .
O1 Co1 O3 C12 71.29(18) . .
N1 Co1 O3 C12 164.61(18) . .
N3 Co1 O3 C12 -19.77(18) . .
N4 Co1 O3 C12 -78(2) . .
N2 Co1 O3 C12 -111.04(18) . .
N5 O5 O6 O7 98(2) . .
N5 O5 O6 N6 112.2(13) . 2_666
O5 O6 O7 C49 97(3) . 2_666
N6 O6 O7 C49 74(2) 2_666 2_666
O5 O6 O7 N6 23(2) . 2_666
O5 O6 O7 C50 135.4(19) . 2_666
N6 O6 O7 C50 112.8(16) 2_666 2_666
O1 Co1 N1 C7 -14.7(2) . .
O3 Co1 N1 C7 -105.0(2) . .
N3 Co1 N1 C7 137.3(9) . .
N4 Co1 N1 C7 76.5(2) . .
N2 Co1 N1 C7 168.4(2) . .
O1 Co1 N1 C8 155.82(15) . .
O3 Co1 N1 C8 65.52(15) . .
N3 Co1 N1 C8 -52.2(10) . .
N4 Co1 N1 C8 -112.98(15) . .
N2 Co1 N1 C8 -21.04(15) . .
O1 Co1 N2 C9 -58.0(11) . .
O3 Co1 N2 C9 -93.71(15) . .
N1 Co1 N2 C9 -5.87(15) . .
N3 Co1 N2 C9 171.58(15) . .
N4 Co1 N2 C9 87.22(15) . .
O1 Co1 N3 C18 -85.0(2) . .
O3 Co1 N3 C18 5.5(2) . .
N1 Co1 N3 C18 122.9(9) . .
N4 Co1 N3 C18 -175.9(2) . .
N2 Co1 N3 C18 91.9(2) . .
O1 Co1 N3 C19 103.04(17) . .
O3 Co1 N3 C19 -166.43(16) . .
N1 Co1 N3 C19 -49.0(10) . .
N4 Co1 N3 C19 12.13(16) . .
N2 Co1 N3 C19 -79.98(17) . .
O1 Co1 N4 C20 -79.30(15) . .
O3 Co1 N4 C20 70(2) . .
N1 Co1 N4 C20 -172.71(15) . .
N3 Co1 N4 C20 11.62(15) . .
N2 Co1 N4 C20 102.97(15) . .
O6 O5 N5 C47 169(6) . .
Co1 O1 C1 C2 156.45(17) . .
Co1 O1 C1 C6 -26.5(3) . .
O1 C1 C2 C3 178.4(2) . .
C6 C1 C2 C3 1.1(4) . .
C1 C2 C3 C4 0.1(4) . .
C2 C3 C4 C5 -1.1(5) . .
C3 C4 C5 C6 0.9(4) . .
C4 C5 C6 C1 0.3(4) . .
C4 C5 C6 C7 -174.7(2) . .
O1 C1 C6 C5 -178.3(2) . .
C2 C1 C6 C5 -1.3(3) . .
O1 C1 C6 C7 -3.7(3) . .
C2 C1 C6 C7 173.4(2) . .
C8 N1 C7 O2 3.7(3) . .
Co1 N1 C7 O2 173.72(16) . .
C8 N1 C7 C6 -176.72(18) . .
Co1 N1 C7 C6 -6.7(3) . .
C5 C6 C7 O2 15.3(3) . .
C1 C6 C7 O2 -159.5(2) . .
C5 C6 C7 N1 -164.4(2) . .
C1 C6 C7 N1 20.9(3) . .
C7 N1 C8 C9 -145.15(19) . .
Co1 N1 C8 C9 43.1(2) . .
Co1 N2 C9 C11 149.80(17) . .
Co1 N2 C9 C8 29.2(2) . .
Co1 N2 C9 C10 -89.47(19) . .
N1 C8 C9 N2 -45.2(2) . .
N1 C8 C9 C11 -164.8(2) . .
N1 C8 C9 C10 72.4(2) . .
Co1 O3 C12 C13 -160.20(15) . .
Co1 O3 C12 C17 22.2(3) . .
O3 C12 C13 C14 -176.2(2) . .
C17 C12 C13 C14 1.6(3) . .
C12 C13 C14 C15 0.7(3) . .
C13 C14 C15 C16 -1.6(4) . .
C14 C15 C16 C17 0.1(4) . .
C15 C16 C17 C12 2.2(4) . .
C15 C16 C17 C18 -178.1(2) . .
O3 C12 C17 C16 174.6(2) . .
C13 C12 C17 C16 -3.0(3) . .
O3 C12 C17 C18 -5.0(4) . .
C13 C12 C17 C18 177.4(2) . .
C19 N3 C18 O4 -1.5(4) . .
Co1 N3 C18 O4 -173.23(19) . .
C19 N3 C18 C17 179.0(2) . .
Co1 N3 C18 C17 7.3(3) . .
C16 C17 C18 O4 -9.8(3) . .
C12 C17 C18 O4 169.9(2) . .
C16 C17 C18 N3 169.7(2) . .
C12 C17 C18 N3 -10.6(4) . .
C18 N3 C19 C20 154.0(2) . .
Co1 N3 C19 C20 -33.0(2) . .
Co1 N4 C20 C22 88.8(2) . .
Co1 N4 C20 C19 -30.9(2) . .
Co1 N4 C20 C21 -150.17(17) . .
N3 C19 C20 N4 39.9(2) . .
N3 C19 C20 C22 -77.9(2) . .
N3 C19 C20 C21 158.5(2) . .
C35 P1 C23 C28 -29.9(2) . .
C41 P1 C23 C28 89.3(2) . .
C29 P1 C23 C28 -152.94(19) . .
C35 P1 C23 C24 153.03(18) . .
C41 P1 C23 C24 -87.81(19) . .
C29 P1 C23 C24 30.0(2) . .
C28 C23 C24 C25 -1.5(3) . .
P1 C23 C24 C25 175.53(18) . .
C23 C24 C25 C26 0.8(4) . .
C24 C25 C26 C27 0.5(4) . .
C25 C26 C27 C28 -1.1(4) . .
C26 C27 C28 C23 0.4(4) . .
C24 C23 C28 C27 0.9(4) . .
P1 C23 C28 C27 -176.2(2) . .
C35 P1 C29 C34 116.29(18) . .
C23 P1 C29 C34 -123.23(18) . .
C41 P1 C29 C34 -4.8(2) . .
C35 P1 C29 C30 -63.4(2) . .
C23 P1 C29 C30 57.07(19) . .
C41 P1 C29 C30 175.48(17) . .
C34 C29 C30 C31 -2.8(3) . .
P1 C29 C30 C31 176.91(17) . .
C29 C30 C31 C32 2.3(4) . .
C30 C31 C32 C33 0.3(4) . .
C31 C32 C33 C34 -2.5(4) . .
C32 C33 C34 C29 2.0(3) . .
C30 C29 C34 C33 0.6(3) . .
P1 C29 C34 C33 -179.05(17) . .
C23 P1 C35 C40 104.2(2) . .
C41 P1 C35 C40 -15.0(2) . .
C29 P1 C35 C40 -135.50(19) . .
C23 P1 C35 C36 -71.6(2) . .
C41 P1 C35 C36 169.25(19) . .
C29 P1 C35 C36 48.7(2) . .
C40 C35 C36 C37 -2.5(4) . .
P1 C35 C36 C37 173.3(2) . .
C35 C36 C37 C38 0.4(4) . .
C36 C37 C38 C39 2.2(4) . .
C37 C38 C39 C40 -2.6(4) . .
C38 C39 C40 C35 0.5(4) . .
C36 C35 C40 C39 2.1(4) . .
P1 C35 C40 C39 -173.67(19) . .
C35 P1 C41 C46 127.37(19) . .
C23 P1 C41 C46 8.6(2) . .
C29 P1 C41 C46 -109.29(19) . .
C35 P1 C41 C42 -55.2(2) . .
C23 P1 C41 C42 -174.01(17) . .
C29 P1 C41 C42 68.13(19) . .
C46 C41 C42 C43 1.2(3) . .
P1 C41 C42 C43 -176.27(17) . .
C41 C42 C43 C44 -0.8(3) . .
C42 C43 C44 C45 0.1(4) . .
C43 C44 C45 C46 0.3(4) . .
C42 C41 C46 C45 -0.7(3) . .
P1 C41 C46 C45 176.67(19) . .
C44 C45 C46 C41 0.0(4) . .
O5 N5 C47 C48 52(9) . .
O6 N6 C49 O7 -51.3(17) 2_666 2_666
O7 N6 C49 C50 62(3) 2_666 .
O6 N6 C49 C50 11(3) 2_666 .
N6 C49 C50 O7 -46(3) . 2_666
