#------------------------------------------------------------------------------
#$Date: 2014-07-12 01:16:09 +0300 (Sat, 12 Jul 2014) $
#$Revision: 120081 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/00/4300097.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_4300097
loop_
_publ_author_name
'Laurie A. Tyler'
'Juan C. Noveron'
'Marilyn M. Olmstead'
'Pradip K. Mascharak'
_publ_contact_author
; Pradip K. Mascharak
  Department of Chemistry and Biochemistry
  University of California
  Santa Cruz, CA 95064
  USA
;
_publ_contact_author_email       mascharak@chemistry.ucsc.edu
_publ_contact_author_fax         831-459-2935
_publ_contact_author_phone       831-459-4251
_publ_section_title
;
Co(III) Complexes with Coordinated Carboxamido Nitrogens and Thiolato
Sulfurs as Models for Co-Containing Nitrile Hydratase and Their Conversion
to the Corresponding Sulfinato Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              357
_journal_page_last               362
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C21 H30 Co N4 Na O8 S2'
_chemical_formula_weight         612.53
_chemical_name_common            Na[Co(PyPePRSO2)2].H2O.CH3OH
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 100.481(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7489(11)
_cell_length_b                   13.1151(13)
_cell_length_c                   20.998(3)
_cell_measurement_reflns_used    138
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     2640.0(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL v. 5.03, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_sigmaI/netI    0.0970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13256
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        <0.1
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.8441
_exptl_absorpt_correction_T_min  0.7913
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS, Sheldrick, G.M., an empirical absorption correction program based 
 on the method of Blessing, R. H., Acta Cryst. (1995). A51, 33-38.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         3806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0584P)²+2.0189P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                2333
_reflns_number_total             3806
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        2640.0(5)
_cod_database_code               4300097
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.37402(8) 0.80821(5) 0.11966(3) 0.0211(2) Uani 1 1 d . A .
Na Na 0.1115(2) 0.95710(16) -0.06346(10) 0.0340(6) Uani 1 1 d . . .
S1 S 0.32924(15) 0.75494(11) 0.01885(6) 0.0270(4) Uani 1 1 d . A .
S2 S 0.21702(15) 0.93319(10) 0.11236(6) 0.0248(3) Uani 1 1 d . A .
O1 O 0.1267(5) 0.6479(3) 0.21527(19) 0.0539(13) Uani 1 1 d . . .
O2 O 0.4517(4) 0.7078(3) 0.00106(17) 0.0467(12) Uani 1 1 d . . .
O3 O 0.2616(4) 0.8270(3) -0.02952(17) 0.0377(10) Uani 1 1 d . . .
O4 O 0.7235(4) 0.9388(3) 0.0840(2) 0.0436(11) Uani 1 1 d . . .
O5 O 0.1585(4) 0.9390(3) 0.17226(17) 0.0365(10) Uani 1 1 d . . .
O6 O 0.1079(4) 0.9403(3) 0.05375(17) 0.0334(10) Uani 1 1 d . . .
N1 N 0.4101(4) 0.8178(3) 0.21649(19) 0.0226(10) Uani 1 1 d . A .
N2 N 0.2423(5) 0.7086(3) 0.13628(19) 0.0252(11) Uani 1 1 d . . .
N3 N 0.5469(5) 0.7246(3) 0.13387(18) 0.0225(11) Uani 1 1 d . . .
N4 N 0.4995(5) 0.9114(3) 0.10094(19) 0.0219(11) Uani 1 1 d . . .
C1 C 0.5152(6) 0.8628(4) 0.2548(3) 0.0283(14) Uani 1 1 d . . .
H1 H 0.5821 0.8963 0.2362 0.034 Uiso 1 1 calc R . .
C2 C 0.5299(7) 0.8622(4) 0.3218(3) 0.0365(16) Uani 1 1 d . . .
H2 H 0.6052 0.8940 0.3478 0.044 Uiso 1 1 calc R . .
C3 C 0.4291(7) 0.8127(5) 0.3485(3) 0.0393(16) Uani 1 1 d . . .
H3 H 0.4327 0.8141 0.3930 0.047 Uiso 1 1 calc R . .
C4 C 0.3243(7) 0.7617(4) 0.3096(3) 0.0368(16) Uani 1 1 d . A .
H4 H 0.2580 0.7264 0.3276 0.044 Uiso 1 1 calc R . .
C5 C 0.3169(6) 0.7627(4) 0.2433(2) 0.0268(13) Uani 1 1 d . . .
C6 C 0.2174(6) 0.7023(4) 0.1965(3) 0.0306(14) Uani 1 1 d . A .
C7A C 0.1390(9) 0.6732(6) 0.0813(3) 0.028(2) Uiso 0.737(9) 1 d P A 1
H7A1 H 0.0681 0.7253 0.0700 0.034 Uiso 0.737(9) 1 calc PR A 1
H7A2 H 0.0939 0.6124 0.0938 0.034 Uiso 0.737(9) 1 calc PR A 1
C9A C 0.1033(10) 0.6431(7) -0.0386(4) 0.049(3) Uiso 0.737(9) 1 d P A 1
H9A1 H 0.1539 0.6279 -0.0726 0.074 Uiso 0.737(9) 1 calc PR A 1
H9A2 H 0.0555 0.7069 -0.0475 0.074 Uiso 0.737(9) 1 calc PR A 1
H9A3 H 0.0367 0.5900 -0.0361 0.074 Uiso 0.737(9) 1 calc PR A 1
C10A C 0.2933(9) 0.5462(6) 0.0345(4) 0.048(3) Uiso 0.737(9) 1 d P A 1
H10D H 0.3339 0.5334 -0.0031 0.072 Uiso 0.737(9) 1 calc PR A 1
H10E H 0.2341 0.4902 0.0411 0.072 Uiso 0.737(9) 1 calc PR A 1
H10F H 0.3660 0.5536 0.0718 0.072 Uiso 0.737(9) 1 calc PR A 1
C7B C 0.193(3) 0.6228(18) 0.0890(10) 0.034(6) Uiso 0.263(9) 1 d P A 2
H7B1 H 0.2491 0.5626 0.1015 0.040 Uiso 0.263(9) 1 calc PR A 2
H7B2 H 0.0968 0.6062 0.0912 0.040 Uiso 0.263(9) 1 calc PR A 2
C9B C 0.034(3) 0.715(2) -0.0004(14) 0.073(10) Uiso 0.263(9) 1 d P A 2
H9B1 H 0.0261 0.7688 0.0297 0.109 Uiso 0.263(9) 1 calc PR A 2
H9B2 H -0.0404 0.6672 -0.0009 0.109 Uiso 0.263(9) 1 calc PR A 2
H9B3 H 0.0289 0.7435 -0.0430 0.109 Uiso 0.263(9) 1 calc PR A 2
C10B C 0.185(3) 0.577(2) -0.0267(13) 0.059(9) Uiso 0.263(9) 1 d P A 2
H10A H 0.2007 0.6088 -0.0659 0.088 Uiso 0.263(9) 1 calc PR A 2
H10B H 0.0923 0.5497 -0.0330 0.088 Uiso 0.263(9) 1 calc PR A 2
H10C H 0.2513 0.5228 -0.0153 0.088 Uiso 0.263(9) 1 calc PR A 2
C8 C 0.2020(7) 0.6501(4) 0.0239(3) 0.0394(16) Uani 1 1 d . . .
C11 C 0.5667(6) 0.6300(4) 0.1559(3) 0.0320(14) Uani 1 1 d . A .
H11 H 0.4912 0.5946 0.1665 0.038 Uiso 1 1 calc R . .
C12 C 0.6926(7) 0.5826(4) 0.1639(3) 0.0402(16) Uani 1 1 d . . .
H12 H 0.7018 0.5157 0.1787 0.048 Uiso 1 1 calc R A .
C13 C 0.8053(7) 0.6337(5) 0.1499(3) 0.0486(18) Uani 1 1 d . A .
H13 H 0.8920 0.6021 0.1543 0.058 Uiso 1 1 calc R . .
C14 C 0.7873(6) 0.7343(5) 0.1289(3) 0.0383(15) Uani 1 1 d . . .
H14 H 0.8626 0.7718 0.1200 0.046 Uiso 1 1 calc R A .
C15 C 0.6582(6) 0.7770(4) 0.1213(2) 0.0270(14) Uani 1 1 d . A .
C16 C 0.6286(6) 0.8851(4) 0.0994(2) 0.0267(14) Uani 1 1 d . A .
C17 C 0.4440(6) 1.0103(4) 0.0755(3) 0.0283(14) Uani 1 1 d . A .
H17A H 0.4068 1.0038 0.0295 0.034 Uiso 1 1 calc R . .
H17B H 0.5190 1.0599 0.0807 0.034 Uiso 1 1 calc R . .
C18 C 0.3310(6) 1.0472(4) 0.1099(2) 0.0266(14) Uani 1 1 d . . .
C19 C 0.2473(7) 1.1353(4) 0.0733(3) 0.0405(16) Uani 1 1 d . A .
H19A H 0.3089 1.1910 0.0692 0.061 Uiso 1 1 calc R . .
H19B H 0.1769 1.1573 0.0968 0.061 Uiso 1 1 calc R . .
H19C H 0.2038 1.1124 0.0310 0.061 Uiso 1 1 calc R . .
C20 C 0.3864(7) 1.0801(4) 0.1799(3) 0.0443(17) Uani 1 1 d . A .
H20A H 0.4496 1.1363 0.1801 0.066 Uiso 1 1 calc R . .
H20B H 0.4344 1.0240 0.2035 0.066 Uiso 1 1 calc R . .
H20C H 0.3098 1.1007 0.1999 0.066 Uiso 1 1 calc R . .
O7 O 0.0238(5) 0.8963(3) -0.16972(19) 0.0532(13) Uani 1 1 d . . .
H7C H -0.0374 0.9507 -0.1817 0.050 Uiso 1 1 d . . .
H7D H 0.0356 0.8764 -0.2088 0.050 Uiso 1 1 d . . .
O8 O 0.1541(10) 0.4400(6) 0.1883(5) 0.167(4) Uani 1 1 d . . .
H8 H 0.1056 0.4882 0.1730 0.050 Uiso 1 1 calc R . .
C21 C 0.0756(11) 0.3737(7) 0.2167(5) 0.109(4) Uani 1 1 d . . .
H21A H 0.0960 0.3827 0.2628 0.163 Uiso 1 1 calc R . .
H21B H 0.0971 0.3050 0.2061 0.163 Uiso 1 1 calc R . .
H21C H -0.0216 0.3869 0.2011 0.163 Uiso 1 1 calc R . .
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'
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'
Na Na 0.0362 0.0249 '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
N2 Co N4 177.51(19) . . ?
N2 Co N3 100.09(18) . . ?
N4 Co N3 82.23(18) . . ?
N2 Co N1 81.80(17) . . ?
N4 Co N1 99.39(18) . . ?
N3 Co N1 83.96(16) . . ?
N2 Co S1 86.34(13) . . ?
N4 Co S1 92.83(13) . . ?
N3 Co S1 89.06(12) . . ?
N1 Co S1 164.95(14) . . ?
N2 Co S2 92.26(14) . . ?
N4 Co S2 85.55(13) . . ?
N3 Co S2 165.75(13) . . ?
N1 Co S2 90.86(13) . . ?
S1 Co S2 98.86(6) . . ?
O4 Na O3 94.29(17) 3_675 . ?
O4 Na O7 100.02(18) 3_675 . ?
O3 Na O7 98.24(16) . . ?
O4 Na O6 113.03(16) 3_675 . ?
O3 Na O6 75.33(14) . . ?
O7 Na O6 146.59(17) . . ?
O4 Na O6 109.75(16) 3_675 3_575 ?
O3 Na O6 149.99(16) . 3_575 ?
O7 Na O6 95.04(15) . 3_575 ?
O6 Na O6 78.77(14) . 3_575 ?
O4 Na Na 118.10(15) 3_675 3_575 ?
O3 Na Na 114.14(13) . 3_575 ?
O7 Na Na 126.04(15) . 3_575 ?
O6 Na Na 40.21(9) . 3_575 ?
O6 Na Na 38.56(9) 3_575 3_575 ?
O2 S1 O3 112.7(2) . . ?
O2 S1 C8 106.7(3) . . ?
O3 S1 C8 107.3(3) . . ?
O2 S1 Co 110.78(17) . . ?
O3 S1 Co 116.86(16) . . ?
C8 S1 Co 101.37(18) . . ?
O5 S2 O6 112.1(2) . . ?
O5 S2 C18 107.9(2) . . ?
O6 S2 C18 105.6(2) . . ?
O5 S2 Co 110.27(16) . . ?
O6 S2 Co 119.04(16) . . ?
C18 S2 Co 100.73(18) . . ?
S1 O3 Na 152.8(2) . . ?
C16 O4 Na 175.1(4) . 3_675 ?
S2 O6 Na 134.1(2) . . ?
S2 O6 Na 116.8(2) . 3_575 ?
Na O6 Na 101.23(14) . 3_575 ?
C1 N1 C5 119.2(4) . . ?
C1 N1 Co 128.3(4) . . ?
C5 N1 Co 112.3(3) . . ?
C6 N2 C7A 120.8(5) . . ?
C6 N2 C7B 118.9(9) . . ?
C7A N2 C7B 32.7(9) . . ?
C6 N2 Co 117.4(4) . . ?
C7A N2 Co 117.5(4) . . ?
C7B N2 Co 122.1(9) . . ?
C11 N3 C15 118.3(5) . . ?
C11 N3 Co 129.4(4) . . ?
C15 N3 Co 112.3(3) . . ?
C16 N4 C17 121.0(4) . . ?
C16 N4 Co 118.2(4) . . ?
C17 N4 Co 119.5(3) . . ?
N1 C1 C2 122.7(6) . . ?
C3 C2 C1 117.7(6) . . ?
C4 C3 C2 120.0(5) . . ?
C3 C4 C5 119.7(6) . . ?
N1 C5 C4 120.4(5) . . ?
N1 C5 C6 114.6(4) . . ?
C4 C5 C6 124.9(5) . . ?
O1 C6 N2 126.4(5) . . ?
O1 C6 C5 120.7(5) . . ?
N2 C6 C5 112.8(5) . . ?
N2 C7A C8 112.3(6) . . ?
C8 C7B N2 111.8(15) . . ?
C7B C8 C10B 121.8(15) . . ?
C7B C8 C7A 33.5(10) . . ?
C10B C8 C7A 137.7(12) . . ?
C7B C8 C9A 133.4(11) . . ?
C10B C8 C9A 47.7(12) . . ?
C7A C8 C9A 115.8(7) . . ?
C7B C8 C10A 77.7(11) . . ?
C10B C8 C10A 61.3(12) . . ?
C7A C8 C10A 111.1(6) . . ?
C9A C8 C10A 108.8(6) . . ?
C7B C8 C9B 100.1(15) . . ?
C10B C8 C9B 97.5(15) . . ?
C7A C8 C9B 69.5(10) . . ?
C9A C8 C9B 51.6(10) . . ?
C10A C8 C9B 150.4(10) . . ?
C7B C8 S1 113.3(9) . . ?
C10B C8 S1 116.3(11) . . ?
C7A C8 S1 105.8(4) . . ?
C9A C8 S1 109.0(5) . . ?
C10A C8 S1 105.8(5) . . ?
C9B C8 S1 102.1(10) . . ?
N3 C11 C12 122.8(6) . . ?
C11 C12 C13 119.6(6) . . ?
C12 C13 C14 118.3(6) . . ?
C15 C14 C13 119.2(6) . . ?
N3 C15 C14 121.8(5) . . ?
N3 C15 C16 115.1(5) . . ?
C14 C15 C16 123.1(5) . . ?
O4 C16 N4 128.0(5) . . ?
O4 C16 C15 120.1(5) . . ?
N4 C16 C15 111.9(5) . . ?
N4 C17 C18 111.3(4) . . ?
C17 C18 C20 113.0(5) . . ?
C17 C18 C19 111.8(4) . . ?
C20 C18 C19 109.3(4) . . ?
C17 C18 S2 104.3(3) . . ?
C20 C18 S2 107.8(4) . . ?
C19 C18 S2 110.5(4) . . ?
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 N2 1.908(4) . ?
Co N4 1.912(4) . ?
Co N3 1.987(4) . ?
Co N1 2.003(4) . ?
Co S1 2.1962(15) . ?
Co S2 2.2288(16) . ?
Na O4 2.211(4) 3_675 ?
Na O3 2.277(4) . ?
Na O7 2.377(5) . ?
Na O6 2.478(4) . ?
Na O6 2.566(4) 3_575 ?
Na Na 3.899(4) 3_575 ?
S1 O2 1.452(4) . ?
S1 O3 1.454(4) . ?
S1 C8 1.868(6) . ?
S2 O5 1.474(4) . ?
S2 O6 1.476(4) . ?
S2 C18 1.870(5) . ?
O1 C6 1.254(6) . ?
O4 C16 1.252(6) . ?
O4 Na 2.211(4) 3_675 ?
O6 Na 2.566(4) 3_575 ?
N1 C1 1.322(7) . ?
N1 C5 1.361(6) . ?
N2 C6 1.333(6) . ?
N2 C7A 1.462(8) . ?
N2 C7B 1.52(2) . ?
N3 C11 1.325(6) . ?
N3 C15 1.351(7) . ?
N4 C16 1.312(7) . ?
N4 C17 1.468(6) . ?
C1 C2 1.387(7) . ?
C2 C3 1.379(8) . ?
C3 C4 1.362(8) . ?
C4 C5 1.381(7) . ?
C5 C6 1.479(7) . ?
C7A C8 1.480(9) . ?
C9A C8 1.482(10) . ?
C10A C8 1.620(10) . ?
C7B C8 1.43(2) . ?
C9B C8 1.83(3) . ?
C10B C8 1.42(3) . ?
C11 C12 1.359(8) . ?
C12 C13 1.363(8) . ?
C13 C14 1.393(8) . ?
C14 C15 1.360(8) . ?
C15 C16 1.501(7) . ?
C17 C18 1.503(7) . ?
C18 C20 1.533(7) . ?
C18 C19 1.536(7) . ?
O8 C21 1.365(10) . ?
_journal_paper_doi 10.1021/ic990794m
