#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:00:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179166 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/27/4312775.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_4312775
loop_
_publ_author_name
'Dong Mok Shin'
'In Su Lee'
'Young Keun Chung'
_publ_section_title
;
 Self-Assemblies of New Rigid Angular Ligands and Metal Centers toward the
 Rational Construction and Modification of Novel Coordination Polymer
 Networks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8838
_journal_page_last               8846
_journal_paper_doi               10.1021/ic0345929
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C33 H29 Co N7 O6 S2'
_chemical_formula_weight         742.68
_chemical_name_systematic
; 
 ? 
;
_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                 104.4352(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.54000(10)
_cell_length_b                   23.5649(5)
_cell_length_c                   16.6758(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.62
_cell_measurement_theta_min      2.80
_cell_volume                     3630.52(11)
_computing_cell_refinement       DenzoSMN
_computing_data_collection       DenzoSMN
_computing_data_reduction        DenzoSMN
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0807
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20105
_diffrn_reflns_theta_full        26.62
_diffrn_reflns_theta_max         26.62
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.639
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7432
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1492
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.953
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1661P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2217
_refine_ls_wR_factor_ref         0.2583
_reflns_number_gt                3552
_reflns_number_total             7432
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0345929si20030529_081404_4.cif
_cod_data_source_block           compound4
_cod_database_code               4312775
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 -0.18406(7) 0.27188(3) 0.10512(5) 0.0612(3) Uani 1 1 d . . .
S1 S -0.64813(18) 0.26025(12) 0.14880(13) 0.1134(8) Uani 1 1 d . . .
S2 S -0.2638(3) 0.43783(9) -0.05620(17) 0.1448(10) Uani 1 1 d . . .
N1 N -0.1011(4) 0.20453(18) 0.0556(3) 0.0570(10) Uani 1 1 d . . .
N2 N -0.0296(4) 0.29264(18) 0.2092(3) 0.0588(11) Uani 1 1 d . . .
N3 N -0.3725(5) 0.2567(2) 0.1252(3) 0.0755(13) Uani 1 1 d . . .
N4 N -0.2059(5) 0.3404(2) 0.0368(3) 0.0786(14) Uani 1 1 d . . .
C1 C 0.0154(5) 0.1788(2) 0.1017(3) 0.0667(14) Uani 1 1 d . . .
H1 H 0.0553 0.1927 0.1546 0.080 Uiso 1 1 calc R . .
C2 C 0.0810(5) 0.1323(2) 0.0750(4) 0.0691(15) Uani 1 1 d . . .
H2 H 0.1630 0.1164 0.1101 0.083 Uiso 1 1 calc R . .
C3 C 0.0268(5) 0.1093(2) -0.0022(3) 0.0555(12) Uani 1 1 d . . .
C4 C -0.0984(5) 0.1367(2) -0.0545(3) 0.0537(12) Uani 1 1 d . . .
C5 C -0.1586(5) 0.1844(2) -0.0225(3) 0.0522(12) Uani 1 1 d . . .
C6 C -0.2814(5) 0.2113(2) -0.0731(4) 0.0633(13) Uani 1 1 d . . .
H6 H -0.3233 0.2418 -0.0524 0.076 Uiso 1 1 calc R . .
C7 C -0.3389(6) 0.1930(3) -0.1518(4) 0.0714(15) Uani 1 1 d . . .
H7 H -0.4181 0.2118 -0.1850 0.086 Uiso 1 1 calc R . .
C8 C -0.2797(6) 0.1459(3) -0.1834(4) 0.0697(15) Uani 1 1 d . . .
H8 H -0.3207 0.1334 -0.2369 0.084 Uiso 1 1 calc R . .
C9 C -0.1628(6) 0.1188(2) -0.1358(3) 0.0625(13) Uani 1 1 d . . .
H9 H -0.1245 0.0878 -0.1575 0.075 Uiso 1 1 calc R . .
C10 C 0.0945(5) 0.0600(2) -0.0304(3) 0.0638(14) Uani 1 1 d . . .
H10 H 0.0586 0.0486 -0.0851 0.077 Uiso 1 1 calc R . .
C11 C 0.2031(6) 0.0304(2) 0.0159(4) 0.0659(14) Uani 1 1 d . . .
H11 H 0.2349 0.0419 0.0708 0.079 Uiso 1 1 calc R . .
C12 C 0.2789(5) -0.0179(2) -0.0081(3) 0.0579(13) Uani 1 1 d . . .
C13 C 0.2443(7) -0.0390(3) -0.0893(4) 0.0800(17) Uani 1 1 d . . .
H13 H 0.1697 -0.0226 -0.1294 0.096 Uiso 1 1 calc R . .
C14 C 0.3211(7) -0.0842(3) -0.1099(4) 0.0835(18) Uani 1 1 d . . .
H14 H 0.2957 -0.0987 -0.1634 0.100 Uiso 1 1 calc R . .
C15 C 0.4357(7) -0.1083(2) -0.0515(4) 0.0776(16) Uani 1 1 d . . .
H15 H 0.4884 -0.1378 -0.0667 0.093 Uiso 1 1 calc R . .
C16 C 0.4722(5) -0.0883(2) 0.0300(4) 0.0623(14) Uani 1 1 d . . .
C17 C 0.3909(5) -0.0423(2) 0.0485(3) 0.0617(13) Uani 1 1 d . . .
H17 H 0.4150 -0.0278 0.1021 0.074 Uiso 1 1 calc R . .
C18 C 0.5908(5) -0.1108(2) 0.0939(3) 0.0626(13) Uani 1 1 d . . .
H18 H 0.6072 -0.0926 0.1449 0.075 Uiso 1 1 calc R . .
C19 C 0.0485(6) 0.3387(2) 0.2066(4) 0.0666(14) Uani 1 1 d . . .
H19 H 0.0257 0.3601 0.1582 0.080 Uiso 1 1 calc R . .
C20 C 0.1605(6) 0.3573(2) 0.2699(4) 0.0665(14) Uani 1 1 d . . .
H20 H 0.2096 0.3904 0.2631 0.080 Uiso 1 1 calc R . .
C21 C 0.2013(5) 0.3278(2) 0.3434(3) 0.0591(13) Uani 1 1 d . . .
C22 C 0.1186(5) 0.2779(2) 0.3504(3) 0.0553(13) Uani 1 1 d . . .
C23 C 0.0033(5) 0.2623(2) 0.2824(3) 0.0555(13) Uani 1 1 d . . .
C24 C -0.0808(6) 0.2138(2) 0.2886(4) 0.0651(14) Uani 1 1 d . . .
H24 H -0.1566 0.2034 0.2442 0.078 Uiso 1 1 calc R . .
C25 C -0.0517(7) 0.1825(3) 0.3586(4) 0.0796(17) Uani 1 1 d . . .
H25 H -0.1086 0.1510 0.3623 0.096 Uiso 1 1 calc R . .
C26 C 0.0633(6) 0.1970(3) 0.4258(4) 0.0749(16) Uani 1 1 d . . .
H26 H 0.0836 0.1746 0.4732 0.090 Uiso 1 1 calc R . .
C27 C 0.1445(6) 0.2431(2) 0.4221(4) 0.0669(14) Uani 1 1 d . . .
H27 H 0.2195 0.2524 0.4676 0.080 Uiso 1 1 calc R . .
C28 C 0.3206(5) 0.3466(2) 0.4096(4) 0.0657(14) Uani 1 1 d . . .
H28 H 0.3367 0.3269 0.4594 0.079 Uiso 1 1 calc R . .
C29 C -0.4874(7) 0.2580(3) 0.1338(3) 0.0663(14) Uani 1 1 d . . .
C30 C -0.2309(7) 0.3807(3) 0.0001(4) 0.0797(17) Uani 1 1 d . . .
N01 N 0.3447(14) 0.4239(4) 0.1178(9) 0.160(4) Uani 1 1 d . . .
O01 O 0.2159(10) 0.4172(3) 0.0854(6) 0.176(3) Uani 1 1 d . . .
O02 O 0.3843(15) 0.4409(5) 0.1903(7) 0.233(6) Uani 1 1 d . . .
C01 C 0.4495(8) 0.4141(6) 0.0707(5) 0.223(7) Uani 1 1 d . . .
H01A H 0.4036 0.4174 0.0128 0.267 Uiso 1 1 calc R . .
H01B H 0.4893 0.3767 0.0822 0.267 Uiso 1 1 calc R . .
H01C H 0.5256 0.4417 0.0858 0.267 Uiso 1 1 calc R . .
N02 N 0.0958(7) 0.4950(3) 0.7971(5) 0.378(17) Uani 1 1 d RD . .
O03 O 0.0593(7) 0.4748(3) 0.8739(5) 0.333(8) Uani 1 1 d RD . .
O04 O 0.0175(8) 0.5110(3) 0.7473(5) 0.388(12) Uani 1 1 d RD . .
C02 C 0.1795(8) 0.5372(3) 0.8171(6) 0.55(4) Uani 1 1 d RD . .
N03 N 0.4833(7) 0.3579(3) 0.7790(5) 1.23(11) Uani 1 1 d RD . .
O05 O 0.4104(7) 0.3356(3) 0.8302(5) 0.62(3) Uani 1 1 d RD . .
O06 O 0.4080(7) 0.3937(3) 0.7376(5) 0.58(3) Uani 1 1 d RD . .
C03 C 0.5677(7) 0.3380(3) 0.7800(5) 0.354(17) Uani 1 1 d RD . .
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'
Co Co 0.3494 0.9721 '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'
O O 0.0106 0.0060 '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
N3 Co N4 106.5(2) . . ?
N3 Co N1 113.33(18) . . ?
N4 Co N1 113.7(2) . . ?
N3 Co N2 113.66(18) . . ?
N4 Co N2 104.4(2) . . ?
N1 Co N2 105.12(16) . . ?
C1 N1 C5 118.1(4) . . ?
C1 N1 Co 118.4(3) . . ?
C5 N1 Co 123.6(3) . . ?
C19 N2 C23 116.7(5) . . ?
C19 N2 Co 117.5(4) . . ?
C23 N2 Co 125.8(3) . . ?
C29 N3 Co 167.5(5) . . ?
C30 N4 Co 172.9(5) . . ?
N1 C1 C2 123.7(5) . . ?
C3 C2 C1 121.1(5) . . ?
C2 C3 C4 116.8(5) . . ?
C2 C3 C10 121.4(5) . . ?
C4 C3 C10 121.7(5) . . ?
C9 C4 C5 118.5(5) . . ?
C9 C4 C3 123.1(5) . . ?
C5 C4 C3 118.5(4) . . ?
N1 C5 C6 119.3(5) . . ?
N1 C5 C4 121.8(4) . . ?
C6 C5 C4 118.9(5) . . ?
C7 C6 C5 120.6(5) . . ?
C6 C7 C8 120.5(5) . . ?
C9 C8 C7 120.1(5) . . ?
C8 C9 C4 121.3(5) . . ?
C11 C10 C3 125.0(5) . . ?
C10 C11 C12 128.4(5) . . ?
C17 C12 C13 118.2(5) . . ?
C17 C12 C11 119.8(5) . . ?
C13 C12 C11 121.9(5) . . ?
C14 C13 C12 120.1(6) . . ?
C13 C14 C15 120.9(6) . . ?
C14 C15 C16 120.3(5) . . ?
C15 C16 C17 116.9(5) . . ?
C15 C16 C18 123.5(5) . . ?
C17 C16 C18 119.5(5) . . ?
C12 C17 C16 123.5(5) . . ?
C28 C18 C16 129.5(5) 2_645 . ?
N2 C19 C20 124.9(5) . . ?
C19 C20 C21 121.0(5) . . ?
C20 C21 C22 116.5(5) . . ?
C20 C21 C28 121.3(5) . . ?
C22 C21 C28 122.2(5) . . ?
C23 C22 C27 117.4(5) . . ?
C23 C22 C21 118.7(5) . . ?
C27 C22 C21 123.9(5) . . ?
N2 C23 C24 118.4(5) . . ?
N2 C23 C22 122.2(4) . . ?
C24 C23 C22 119.5(5) . . ?
C25 C24 C23 120.5(6) . . ?
C24 C25 C26 120.6(6) . . ?
C27 C26 C25 120.4(6) . . ?
C26 C27 C22 121.6(6) . . ?
C18 C28 C21 126.1(5) 2_655 . ?
N3 C29 S1 178.3(5) . . ?
N4 C30 S2 177.4(6) . . ?
O01 N01 O02 120.0(13) . . ?
O01 N01 C01 119.9(14) . . ?
O02 N01 C01 120.1(13) . . ?
O04 N02 C02 101.84(6) . . ?
O04 N02 O03 121.9 . . ?
C02 N02 O03 107.0 . . ?
N02 O04 C02 43.6 . . ?
N02 C02 O04 34.52(7) . . ?
C03 N03 O06 138.8 . . ?
C03 N03 O05 112.2 . . ?
O06 N03 O05 108.1 . . ?
N03 O05 C03 27.0 . . ?
N03 C03 O05 40.8 . . ?
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 N3 1.943(5) . ?
Co N4 1.957(6) . ?
Co N1 2.038(4) . ?
Co N2 2.037(4) . ?
S1 C29 1.615(6) . ?
S2 C30 1.628(8) . ?
N1 C1 1.330(6) . ?
N1 C5 1.367(6) . ?
N2 C19 1.324(7) . ?
N2 C23 1.381(6) . ?
N3 C29 1.140(7) . ?
N4 C30 1.122(7) . ?
C1 C2 1.388(7) . ?
C2 C3 1.374(7) . ?
C3 C4 1.443(7) . ?
C3 C10 1.462(7) . ?
C4 C9 1.407(7) . ?
C4 C5 1.425(7) . ?
C5 C6 1.412(7) . ?
C6 C7 1.360(8) . ?
C7 C8 1.406(8) . ?
C8 C9 1.356(7) . ?
C10 C11 1.326(7) . ?
C11 C12 1.456(7) . ?
C12 C17 1.364(7) . ?
C12 C13 1.404(8) . ?
C13 C14 1.383(8) . ?
C14 C15 1.391(8) . ?
C15 C16 1.398(8) . ?
C16 C17 1.411(7) . ?
C16 C18 1.447(7) . ?
C18 C28 1.323(7) 2_645 ?
C19 C20 1.374(7) . ?
C20 C21 1.378(7) . ?
C21 C22 1.436(7) . ?
C21 C28 1.444(7) . ?
C22 C23 1.418(7) . ?
C22 C27 1.420(8) . ?
C23 C24 1.415(7) . ?
C24 C25 1.349(8) . ?
C25 C26 1.401(9) . ?
C26 C27 1.345(8) . ?
C28 C18 1.323(7) 2_655 ?
N01 O01 1.223(12) . ?
N01 O02 1.240(13) . ?
N01 C01 1.435(12) . ?
N02 O04 1.0399 . ?
N02 C02 1.2665(13) . ?
N02 O03 1.4870 . ?
O04 C02 1.7960(12) . ?
N03 C03 0.9284 . ?
N03 O06 1.2079 . ?
N03 O05 1.3358 . ?
O05 C03 1.8925 . ?
