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#$Date: 2016-03-24 02:54:37 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179603 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/67/4506761.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_4506761
loop_
_publ_author_name
'Manna, Paulami'
'Tripuramallu, Bharat Kumar'
'Das, Samar K.'
_publ_section_title
;
 Synthesis, Structural Characterization, and Magnetic Properties of a New
 Series of Coordination Polymers: Importance of Steric Hindrance at the
 Coordination Sphere
;
_journal_issue                   9
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4607
_journal_paper_doi               10.1021/cg300800h
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C23 H17 Co N2 O5'
_chemical_formula_sum            'C23 H17 Co N2 O5'
_chemical_formula_weight         460.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 111.037(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8015(18)
_cell_length_b                   9.1393(12)
_cell_length_c                   17.045(2)
_cell_measurement_temperature    273(2)
_cell_volume                     2006.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20208
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_T_max  0.9159
_exptl_absorpt_correction_T_min  0.7752
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0724P)²+1.9618P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1443
_reflns_number_gt                3497
_reflns_number_total             3925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300800h_si_002.cif
_cod_data_source_block           compound-3
_cod_original_cell_volume        2006.7(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4506761
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.08292(3) 0.89759(5) 1.02824(3) 0.03149(17) Uani 1 1 d .
O2 O -0.03516(18) 0.7564(3) 0.97627(15) 0.0385(6) Uani 1 1 d .
O1 O 0.1308(2) 0.8888(3) 0.92905(15) 0.0406(6) Uani 1 1 d .
O3 O 0.16656(19) 1.0850(2) 1.06324(15) 0.0379(6) Uani 1 1 d .
O5 O 0.1411(3) 1.1032(3) 0.57761(18) 0.0554(8) Uani 1 1 d .
O4 O -0.00320(18) 0.9486(3) 1.10942(15) 0.0361(5) Uani 1 1 d .
N1 N 0.1767(2) 0.7529(3) 1.11568(16) 0.0297(6) Uani 1 1 d .
C20 C -0.1281(3) 0.7913(4) 0.9615(2) 0.0334(7) Uani 1 1 d .
C1 C 0.0740(3) 0.9822(4) 0.8777(2) 0.0320(7) Uani 1 1 d .
C3 C 0.1596(3) 0.9229(4) 0.7746(2) 0.0354(8) Uani 1 1 d .
H3 H 0.1915 0.8436 0.8081 0.043 Uiso 1 1 calc R
C2 C 0.0957(2) 1.0131(3) 0.7999(2) 0.0297(7) Uani 1 1 d .
C21 C -0.1943(3) 0.6803(4) 0.9831(2) 0.0314(7) Uani 1 1 d .
C5 C 0.1308(3) 1.0678(4) 0.6526(2) 0.0381(8) Uani 1 1 d .
C15 C 0.2795(3) 0.7382(4) 1.1364(2) 0.0342(7) Uani 1 1 d .
C22 C -0.1522(3) 0.5474(4) 1.0175(2) 0.0378(8) Uani 1 1 d .
H22 H -0.0864 0.5211 1.0193 0.045 Uiso 1 1 calc R
N2 N 0.3271(3) 0.8314(4) 1.1012(2) 0.0436(8) Uani 1 1 d .
C8 C 0.1961(3) 1.0071(4) 0.5457(2) 0.0407(9) Uani 1 1 d .
C17 C 0.4660(3) 0.9155(4) 1.0534(2) 0.0384(8) Uani 1 1 d .
C11 C 0.1271(3) 0.6596(4) 1.1497(2) 0.0387(8) Uani 1 1 d .
H11 H 0.0559 0.6708 1.1355 0.046 Uiso 1 1 calc R
C23 C -0.2944(3) 0.7143(4) 0.9765(2) 0.0404(8) Uani 1 1 d .
H23 H -0.3246 0.8011 0.9508 0.049 Uiso 1 1 calc R
C7 C 0.0513(3) 1.1332(4) 0.7506(2) 0.0386(8) Uani 1 1 d .
H7 H 0.0087 1.1956 0.7668 0.046 Uiso 1 1 calc R
C16 C 0.4356(3) 0.8184(5) 1.1117(3) 0.0508(10) Uani 1 1 d .
H16A H 0.4501 0.7176 1.1019 0.061 Uiso 1 1 calc R
H16B H 0.4778 0.8427 1.1693 0.061 Uiso 1 1 calc R
C4 C 0.1771(3) 0.9477(4) 0.7012(2) 0.0413(8) Uani 1 1 d .
H4 H 0.2192 0.8850 0.6845 0.050 Uiso 1 1 calc R
C6 C 0.0694(3) 1.1612(4) 0.6781(2) 0.0431(9) Uani 1 1 d .
H6 H 0.0403 1.2433 0.6461 0.052 Uiso 1 1 calc R
C12 C 0.1754(4) 0.5501(5) 1.2035(3) 0.0579(11) Uani 1 1 d .
H12 H 0.1383 0.4873 1.2253 0.069 Uiso 1 1 calc R
C18 C 0.4001(3) 0.9491(4) 0.9741(2) 0.0424(9) Uani 1 1 d .
H18 H 0.3321 0.9151 0.9556 0.051 Uiso 1 1 calc R
C19 C 0.5672(3) 0.9677(4) 1.0788(3) 0.0434(9) Uani 1 1 d .
H19 H 0.6136 0.9459 1.1324 0.052 Uiso 1 1 calc R
C13 C 0.2811(4) 0.5353(5) 1.2246(3) 0.0659(13) Uani 1 1 d .
H13 H 0.3165 0.4617 1.2614 0.079 Uiso 1 1 calc R
C14 C 0.3335(3) 0.6276(5) 1.1920(3) 0.0527(10) Uani 1 1 d .
H14 H 0.4049 0.6178 1.2063 0.063 Uiso 1 1 calc R
C9 C 0.2927(3) 1.0465(4) 0.5493(2) 0.0435(9) Uani 1 1 d .
H9 H 0.3211 1.1356 0.5727 0.052 Uiso 1 1 calc R
C10 C 0.1502(3) 0.8796(4) 0.5078(3) 0.0481(10) Uani 1 1 d .
H10 H 0.0827 0.8569 0.5033 0.058 Uiso 1 1 calc R
H2N H 0.301(3) 0.886(5) 1.080(3) 0.033(12) Uiso 1 1 d .
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'
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
O2 Co1 O1 93.57(10) . .
O2 Co1 O3 162.26(10) . .
O1 Co1 O3 87.55(11) . .
O2 Co1 N1 96.05(10) . .
O1 Co1 N1 105.65(10) . .
O3 Co1 N1 100.69(10) . .
O2 Co1 O4 82.91(9) . .
O1 Co1 O4 163.02(10) . .
O3 Co1 O4 90.87(10) . .
N1 Co1 O4 91.26(10) . .
O2 Co1 Co1 81.20(7) . 3_577
O1 Co1 Co1 101.97(7) . 3_577
O3 Co1 Co1 81.25(7) . 3_577
N1 Co1 Co1 152.37(8) . 3_577
O4 Co1 Co1 61.11(7) . 3_577
C20 O2 Co1 122.1(2) . .
C1 O1 Co1 104.1(2) . .
C20 O3 Co1 122.2(2) 3_577 .
C5 O5 C8 117.8(3) . .
C1 O4 Co1 149.6(2) 3_577 .
C15 N1 C11 118.4(3) . .
C15 N1 Co1 125.8(2) . .
C11 N1 Co1 115.6(2) . .
O3 C20 O2 125.0(3) 3_577 .
O3 C20 C21 118.1(3) 3_577 .
O2 C20 C21 116.7(3) . .
O4 C1 O1 123.2(3) 3_577 .
O4 C1 C2 118.8(3) 3_577 .
O1 C1 C2 118.0(3) . .
C4 C3 C2 121.7(3) . .
C4 C3 H3 119.2 . .
C2 C3 H3 119.2 . .
C7 C2 C3 118.3(3) . .
C7 C2 C1 120.4(3) . .
C3 C2 C1 121.3(3) . .
C23 C21 C22 119.1(3) . .
C23 C21 C20 120.6(3) . .
C22 C21 C20 120.0(3) . .
O5 C5 C6 115.4(3) . .
O5 C5 C4 124.2(3) . .
C6 C5 C4 120.4(3) . .
N1 C15 N2 117.4(3) . .
N1 C15 C14 120.4(3) . .
N2 C15 C14 122.1(3) . .
C9 C22 C21 120.4(3) 4_576 .
C9 C22 H22 119.8 4_576 .
C21 C22 H22 119.8 . .
C15 N2 C16 122.9(3) . .
C15 N2 H2N 119(4) . .
C16 N2 H2N 118(4) . .
C9 C8 C10 121.7(3) . .
C9 C8 O5 118.6(3) . .
C10 C8 O5 119.7(4) . .
C18 C17 C19 117.9(3) . .
C18 C17 C16 122.9(3) . .
C19 C17 C16 119.1(3) . .
N1 C11 C12 123.7(4) . .
N1 C11 H11 118.1 . .
C12 C11 H11 118.1 . .
C10 C23 C21 120.5(3) 4_576 .
C10 C23 H23 119.8 4_576 .
C21 C23 H23 119.8 . .
C6 C7 C2 120.8(3) . .
C6 C7 H7 119.6 . .
C2 C7 H7 119.6 . .
N2 C16 C17 113.1(3) . .
N2 C16 H16A 109.0 . .
C17 C16 H16A 109.0 . .
N2 C16 H16B 109.0 . .
C17 C16 H16B 109.0 . .
H16A C16 H16B 107.8 . .
C3 C4 C5 118.7(3) . .
C3 C4 H4 120.7 . .
C5 C4 H4 120.7 . .
C7 C6 C5 120.0(3) . .
C7 C6 H6 120.0 . .
C5 C6 H6 120.0 . .
C11 C12 C13 117.7(4) . .
C11 C12 H12 121.2 . .
C13 C12 H12 121.2 . .
C17 C18 C19 121.0(3) . 3_677
C17 C18 H18 119.5 . .
C19 C18 H18 119.5 3_677 .
C18 C19 C17 121.1(4) 3_677 .
C18 C19 H19 119.5 3_677 .
C17 C19 H19 119.5 . .
C14 C13 C12 120.2(4) . .
C14 C13 H13 119.9 . .
C12 C13 H13 119.9 . .
C13 C14 C15 119.5(4) . .
C13 C14 H14 120.2 . .
C15 C14 H14 120.2 . .
C8 C9 C22 119.2(3) . 4_675
C8 C9 H9 120.4 . .
C22 C9 H9 120.4 4_675 .
C8 C10 C23 119.0(4) . 4_675
C8 C10 H10 120.5 . .
C23 C10 H10 120.5 4_675 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 2.017(2) .
Co1 O1 2.026(2) .
Co1 O3 2.032(2) .
Co1 N1 2.064(3) .
Co1 O4 2.174(2) .
Co1 Co1 2.8440(9) 3_577
O2 C20 1.256(4) .
O1 C1 1.272(4) .
O3 C20 1.256(4) 3_577
O5 C5 1.375(4) .
O5 C8 1.393(4) .
O4 C1 1.248(4) 3_577
N1 C15 1.340(4) .
N1 C11 1.347(4) .
C20 O3 1.256(4) 3_577
C20 C21 1.496(4) .
C1 O4 1.248(4) 3_577
C1 C2 1.487(4) .
C3 C4 1.376(5) .
C3 C2 1.385(5) .
C3 H3 0.9300 .
C2 C7 1.384(5) .
C21 C23 1.382(5) .
C21 C22 1.383(5) .
C5 C6 1.378(5) .
C5 C4 1.386(5) .
C15 N2 1.342(5) .
C15 C14 1.402(5) .
C22 C9 1.379(5) 4_576
C22 H22 0.9300 .
N2 C16 1.447(5) .
N2 H2N 0.64(4) .
C8 C9 1.361(6) .
C8 C10 1.373(6) .
C17 C18 1.366(5) .
C17 C19 1.391(5) .
C17 C16 1.500(5) .
C11 C12 1.360(5) .
C11 H11 0.9300 .
C23 C10 1.377(5) 4_576
C23 H23 0.9300 .
C7 C6 1.368(5) .
C7 H7 0.9300 .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C4 H4 0.9300 .
C6 H6 0.9300 .
C12 C13 1.378(6) .
C12 H12 0.9300 .
C18 C19 1.373(5) 3_677
C18 H18 0.9300 .
C19 C18 1.373(5) 3_677
C19 H19 0.9300 .
C13 C14 1.355(6) .
C13 H13 0.9300 .
C14 H14 0.9300 .
C9 C22 1.379(5) 4_675
C9 H9 0.9300 .
C10 C23 1.377(5) 4_675
C10 H10 0.9300 .
