#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:09:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179278 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/98/4319855.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_4319855
loop_
_publ_author_name
'Louise Broge'
'Inger Søtofte'
'Carl Erik Olsen'
'Johan Springborg'
_publ_section_title
;
 Cobalt(III) Complexes of [35]Adamanzane,
 1,5,9,13-Tetraazabicyclo[7.7.3]nonadecane. Report of an Inert, Chelate
 Hydrogen Carbonate Ion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3124
_journal_page_last               3129
_journal_paper_doi               10.1021/ic001208o
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C15 H34 As Co F6 N4 O5 S'
_chemical_formula_weight         630.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.356(3)
_cell_length_b                   11.251(2)
_cell_length_c                   15.951(3)
_cell_measurement_temperature    120(2)
_cell_volume                     2217.5(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14601
_diffrn_reflns_theta_max         29.56
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    2.436
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_F_000             1288
_refine_diff_density_max         0.892
_refine_diff_density_min         -1.200
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.097
_refine_ls_goodness_of_fit_obs   1.121
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3031
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.100
_refine_ls_restrained_S_obs      1.125
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_obs          0.0426
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0481P)²+6.8309P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1134
_refine_ls_wR_factor_obs         0.1064
_reflns_number_observed          2580
_reflns_number_total             3031
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001208o_3.cif
_cod_data_source_block           IC001208O-3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+6.8309P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+6.8309P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2217.4(8)
_cod_original_sg_symbol_H-M      'P b m a'
_cod_database_code               4319855
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Co Co 0.18095(4) 0.2500 0.59869(3) 0.01126(14) Uani 1 d S .
S S -0.02512(9) 0.2500 0.60978(7) 0.0190(2) Uani 1 d S .
O1 O 0.0544(2) 0.1476(2) 0.60688(13) 0.0160(4) Uani 1 d . .
O2 O -0.0836(3) 0.2500 0.6876(3) 0.0327(9) Uani 1 d S .
O3 O -0.0951(3) 0.2500 0.5368(3) 0.0334(9) Uani 1 d S .
N1 N 0.2037(3) 0.2500 0.7242(2) 0.0147(7) Uani 1 d S .
H1 H 0.2785(3) 0.2500 0.7311(2) 0.018 Uiso 1 calc SR .
C1 C 0.1662(3) 0.1399(3) 0.7675(2) 0.0189(6) Uani 1 d . .
H11 H 0.0907(3) 0.1220(3) 0.7512(2) 0.023 Uiso 1 calc R .
H12 H 0.1684(3) 0.1517(3) 0.8290(2) 0.023 Uiso 1 calc R .
C2 C 0.2394(3) 0.0374(3) 0.7432(2) 0.0210(6) Uani 1 d . .
H21 H 0.2149(3) -0.0346(3) 0.7734(2) 0.025 Uiso 1 calc R .
H22 H 0.3137(3) 0.0556(3) 0.7626(2) 0.025 Uiso 1 calc R .
C3 C 0.2440(3) 0.0088(3) 0.6502(2) 0.0206(6) Uani 1 d . .
H31 H 0.1706(3) -0.0154(3) 0.6320(2) 0.025 Uiso 1 calc R .
H32 H 0.2922(3) -0.0606(3) 0.6425(2) 0.025 Uiso 1 calc R .
N2 N 0.2827(2) 0.1073(2) 0.5921(2) 0.0142(5) Uani 1 d . .
C4 C 0.2850(3) 0.0501(3) 0.5060(2) 0.0212(6) Uani 1 d . .
H41 H 0.3279(3) 0.1013(3) 0.4679(2) 0.025 Uiso 1 calc R .
H42 H 0.3229(3) -0.0272(3) 0.5103(2) 0.025 Uiso 1 calc R .
C5 C 0.1752(3) 0.0293(3) 0.4668(2) 0.0228(7) Uani 1 d . .
H51 H 0.1268(3) -0.0067(3) 0.5093(2) 0.027 Uiso 1 calc R .
H52 H 0.1830(3) -0.0283(3) 0.4203(2) 0.027 Uiso 1 calc R .
C6 C 0.1226(3) 0.1417(3) 0.4333(2) 0.0208(6) Uani 1 d . .
H61 H 0.1333(3) 0.1460(3) 0.3719(2) 0.025 Uiso 1 calc R .
H62 H 0.0438(3) 0.1389(3) 0.4444(2) 0.025 Uiso 1 calc R .
N3 N 0.1696(3) 0.2500 0.4734(2) 0.0157(7) Uani 1 d S .
H3 H 0.2413(3) 0.2500 0.4556(2) 0.019 Uiso 1 calc SR .
C7 C 0.3980(2) 0.1367(3) 0.6133(2) 0.0212(6) Uani 1 d . .
H71 H 0.4448(2) 0.0700(3) 0.5951(2) 0.025 Uiso 1 calc R .
H72 H 0.4048(2) 0.1437(3) 0.6750(2) 0.025 Uiso 1 calc R .
C8 C 0.4390(4) 0.2500 0.5736(3) 0.0216(9) Uani 1 d S .
H81 H 0.5190(4) 0.2500 0.5762(3) 0.026 Uiso 1 calc SR .
H82 H 0.4180(4) 0.2500 0.5137(3) 0.026 Uiso 1 calc SR .
As As 0.48763(4) 0.2500 0.30760(3) 0.01878(13) Uani 1 d S .
F1 F 0.6214(2) 0.2500 0.2795(2) 0.0334(7) Uani 1 d S .
F2 F 0.3543(3) 0.2500 0.3395(2) 0.0536(12) Uani 1 d S .
F3 F 0.5205(6) 0.1535(7) 0.3932(4) 0.049(2) Uani 0.604(6) d P .
F3' F 0.4933(9) 0.1304(12) 0.3607(5) 0.049(2) Uani 0.396(6) d P .
F4 F 0.4761(5) 0.1193(6) 0.2476(4) 0.062(2) Uani 0.604(6) d P .
F4' F 0.4435(7) 0.1887(9) 0.2208(6) 0.062(2) Uani 0.396(6) d P .
OW O 0.6894(5) 0.2500 0.5171(4) 0.072(2) Uani 1 d SD .
H1OW H 0.7689(25) 0.2500 0.5128 0.086 Uiso 1 d SD .
H2OW H 0.6536(48) 0.2500 0.4600 0.086 Uiso 1 d SD .
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'
S S 0.1246 0.1234 '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'
As As 0.0499 2.0058 '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
_geom_angle_publ_flag
O1 Co O1 72.56(13) . 7_565 ?
O1 Co N3 90.61(11) . . ?
O1 Co N3 90.61(11) 7_565 . ?
O1 Co N1 92.60(10) . . ?
O1 Co N1 92.60(10) 7_565 . ?
N3 Co N1 176.02(15) . . ?
O1 Co N2 164.43(10) . 7_565 ?
O1 Co N2 91.88(10) 7_565 7_565 ?
N3 Co N2 89.53(10) . 7_565 ?
N1 Co N2 88.01(9) . 7_565 ?
O1 Co N2 91.88(10) . . ?
O1 Co N2 164.43(10) 7_565 . ?
N3 Co N2 89.53(10) . . ?
N1 Co N2 88.01(9) . . ?
N2 Co N2 103.69(15) 7_565 . ?
O1 Co S 36.29(6) . . ?
O1 Co S 36.29(7) 7_565 . ?
N3 Co S 89.96(11) . . ?
N1 Co S 94.02(11) . . ?
N2 Co S 128.15(7) 7_565 . ?
N2 Co S 128.15(7) . . ?
O2 S O3 113.2(3) . . ?
O2 S O1 110.67(14) . 7_565 ?
O3 S O1 111.23(14) . 7_565 ?
O2 S O1 110.67(14) . . ?
O3 S O1 111.23(14) . . ?
O1 S O1 99.0(2) 7_565 . ?
O2 S Co 124.2(2) . . ?
O3 S Co 122.6(2) . . ?
O1 S Co 49.52(8) 7_565 . ?
O1 S Co 49.52(8) . . ?
S O1 Co 94.20(11) . . ?
C1 N1 C1 112.2(3) 7_565 . ?
C1 N1 Co 114.5(2) 7_565 . ?
C1 N1 Co 114.5(2) . . ?
N1 C1 C2 109.1(2) . . ?
C1 C2 C3 115.7(3) . . ?
C2 C3 N2 116.9(3) . . ?
C7 N2 C4 106.2(2) . . ?
C7 N2 C3 108.7(2) . . ?
C4 N2 C3 104.4(2) . . ?
C7 N2 Co 113.6(2) . . ?
C4 N2 Co 113.1(2) . . ?
C3 N2 Co 110.4(2) . . ?
C5 C4 N2 115.0(3) . . ?
C4 C5 C6 113.6(3) . . ?
N3 C6 C5 111.3(2) . . ?
C6 N3 C6 109.3(3) . 7_565 ?
C6 N3 Co 117.0(2) . . ?
C6 N3 Co 117.0(2) 7_565 . ?
N2 C7 C8 114.1(3) . . ?
C7 C8 C7 115.1(4) 7_565 . ?
F3' As F3' 115.4(8) 7_565 . ?
F3' As F4' 145.1(7) 7_565 . ?
F3' As F4' 96.2(5) . . ?
F3' As F4' 96.2(5) 7_565 7_565 ?
F3' As F4' 145.1(7) . 7_565 ?
F4' As F4' 49.8(9) . 7_565 ?
F3' As F1 95.5(4) 7_565 . ?
F3' As F1 95.5(4) . . ?
F4' As F1 95.7(3) . . ?
F4' As F1 95.7(3) 7_565 . ?
F3' As F2 83.4(4) 7_565 . ?
F3' As F2 83.4(4) . . ?
F4' As F2 86.1(3) . . ?
F4' As F2 86.1(3) 7_565 . ?
F1 As F2 178.0(2) . . ?
F3' As F4 177.7(5) 7_565 . ?
F3' As F4 65.6(4) . . ?
F4' As F4 33.1(4) . . ?
F4' As F4 82.3(6) 7_565 . ?
F1 As F4 86.3(2) . . ?
F2 As F4 94.8(2) . . ?
F3' As F4 65.6(4) 7_565 7_565 ?
F3' As F4 177.7(5) . 7_565 ?
F4' As F4 82.3(6) . 7_565 ?
F4' As F4 33.1(4) 7_565 7_565 ?
F1 As F4 86.3(2) . 7_565 ?
F2 As F4 94.8(2) . 7_565 ?
F4 As F4 113.3(5) . 7_565 ?
F3' As F3 21.8(5) 7_565 7_565 ?
F3' As F3 95.5(5) . 7_565 ?
F4' As F3 166.9(5) . 7_565 ?
F4' As F3 117.6(4) 7_565 7_565 ?
F1 As F3 88.9(2) . 7_565 ?
F2 As F3 89.5(2) . 7_565 ?
F4 As F3 159.9(4) . 7_565 ?
F4 As F3 85.8(3) 7_565 7_565 ?
F3' As F3 95.5(5) 7_565 . ?
F3' As F3 21.8(5) . . ?
F4' As F3 117.6(4) . . ?
F4' As F3 166.9(6) 7_565 . ?
F1 As F3 88.9(2) . . ?
F2 As F3 89.5(2) . . ?
F4 As F3 85.8(3) . . ?
F4 As F3 159.9(4) 7_565 . ?
F3 As F3 74.6(5) 7_565 . ?
F3' F3 As 62.0(14) . . ?
F3 F3' As 96.2(18) . . ?
F4' F4 As 66.7(6) . . ?
F4 F4' F4' 143.0(6) . 7_565 ?
F4 F4' As 80.2(8) . . ?
F4' F4' As 65.1(4) 7_565 . ?
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
Co O1 1.946(2) . ?
Co O1 1.946(2) 7_565 ?
Co N3 2.003(4) . ?
Co N1 2.022(4) . ?
Co N2 2.042(3) 7_565 ?
Co N2 2.042(3) . ?
Co S 2.5523(13) . ?
S O2 1.436(4) . ?
S O3 1.449(4) . ?
S O1 1.515(2) 7_565 ?
S O1 1.515(2) . ?
N1 C1 1.492(4) 7_565 ?
N1 C1 1.492(4) . ?
C1 C2 1.517(5) . ?
C2 C3 1.519(4) . ?
C3 N2 1.521(4) . ?
N2 C7 1.502(4) . ?
N2 C4 1.518(4) . ?
C4 C5 1.512(5) . ?
C5 C6 1.519(5) . ?
C6 N3 1.494(4) . ?
N3 C6 1.494(4) 7_565 ?
C7 C8 1.511(4) . ?
C8 C7 1.511(4) 7_565 ?
As F3' 1.591(11) 7_565 ?
As F3' 1.591(11) . ?
As F4' 1.640(9) . ?
As F4' 1.640(9) 7_565 ?
As F1 1.712(3) . ?
As F2 1.725(3) . ?
As F4 1.760(5) . ?
As F4 1.760(5) 7_565 ?
As F3 1.792(6) 7_565 ?
As F3 1.792(6) . ?
F3 F3' 0.670(12) . ?
F4 F4' 0.976(11) . ?
F4' F4' 1.38(2) 7_565 ?
