#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/71/4507177.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_4507177
loop_
_publ_author_name
'Kumar, Girijesh'
'Aggarwal, Himanshu'
'Gupta, Rajeev'
_publ_section_title
;
 Cobalt Complexes Appended withpara- andmeta-Arylcarboxylic Acids:
 Influence of Cation, Solvent, and Symmetry on Hydrogen-Bonded Assemblies
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              74
_journal_paper_doi               10.1021/cg3011629
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C13.5 H5 Co0.25 N2.5 O5'
_chemical_formula_weight         296.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   13.137(5)
_cell_length_b                   13.137(5)
_cell_length_c                   15.308(5)
_cell_measurement_reflns_used    2312
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3.08
_cell_volume                     2641.9(17)
_computing_cell_refinement       'X-calibur S SAINT'
_computing_data_collection       'Xcalibur, Sapphire3'
_computing_data_reduction        'X-calibur S SAINT'
_computing_molecular_graphics    'Oxford SHELXTL'
_computing_publication_material  'Oxford SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9597
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1202
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2312
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0964P)²+2.9807P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1671
_reflns_number_gt                2184
_reflns_number_total             2312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg3011629_si_002.cif
_cod_data_source_block           8
_cod_original_formula_sum        'C13.50 H5 Co0.25 N2.50 O5'
_cod_database_code               4507177
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y, x, -z'
'y, -x, -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
C1 C 0.1255(4) 0.3761(4) -0.2053(3) 0.0391(13) Uani 1 1 d .
C2 C 0.0347(4) 0.3269(4) -0.1638(3) 0.0288(10) Uani 1 1 d .
C3 C -0.0631(4) 0.3427(4) -0.1948(4) 0.0358(12) Uani 1 1 d .
H3 H -0.0739 0.3854 -0.2440 0.043 Uiso 1 1 calc R
C4 C -0.1444(4) 0.2967(5) -0.1548(4) 0.0434(14) Uani 1 1 d .
H4 H -0.2113 0.3076 -0.1764 0.052 Uiso 1 1 calc R
C5 C -0.1295(4) 0.2354(4) -0.0841(4) 0.0360(12) Uani 1 1 d .
H5 H -0.1864 0.2044 -0.0565 0.043 Uiso 1 1 calc R
C6 C -0.0326(3) 0.2179(3) -0.0519(3) 0.0225(9) Uani 1 1 d .
C7 C 0.0497(4) 0.2639(4) -0.0921(3) 0.0256(10) Uani 1 1 d .
H7 H 0.1166 0.2523 -0.0707 0.031 Uiso 1 1 calc R
C8 C -0.0162(3) 0.1774(3) 0.1006(3) 0.0235(10) Uani 1 1 d .
C9 C -0.0065(4) 0.0887(3) 0.1622(2) 0.0246(9) Uani 1 1 d .
C10 C -0.0068(5) 0.0920(4) 0.2530(3) 0.0377(12) Uani 1 1 d .
C11 C 0.0000 0.0000 0.2978(4) 0.0463(17) Uani 1 2 d S
C12 C -0.2617(10) 0.3901(10) 0.0994(8) 0.114(4) Uiso 1 1 d .
C13 C -0.3279(18) 0.450(2) -0.0267(17) 0.248(11) Uiso 1 1 d D
C14 C -0.1260(8) 0.4847(9) 0.0239(6) 0.103(3) Uiso 1 1 d D
N1 N -0.0183(2) 0.1457(3) 0.01785(19) 0.0178(7) Uani 1 1 d .
N2 N 0.0000 0.0000 0.1211(3) 0.0215(9) Uani 1 2 d S
N3 N -0.2416(7) 0.4579(7) 0.0289(6) 0.105(3) Uiso 1 1 d D
O1 O -0.0226(3) 0.2665(2) 0.1274(2) 0.0340(9) Uani 1 1 d .
O2 O 0.2065(4) 0.3783(6) -0.1714(4) 0.101(2) Uani 1 1 d .
O1W O -0.3444(13) 0.6270(12) 0.0632(9) 0.206(6) Uiso 1 1 d .
O3 O 0.1054(3) 0.4156(3) -0.2814(2) 0.0435(9) Uani 1 1 d .
H3A H 0.1584 0.4420 -0.3020 0.065 Uiso 1 1 calc R
O4 O -0.213(2) 0.546(2) 0.0510(14) 0.323(11) Uiso 1 1 d .
Co1 Co 0.0000 0.0000 0.0000 0.0175(3) Uani 1 4 d S
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 C1 O3 124.3(5) . .
O2 C1 C2 122.8(5) . .
O3 C1 C2 112.9(5) . .
C3 C2 C7 119.4(4) . .
C3 C2 C1 122.0(4) . .
C7 C2 C1 118.6(4) . .
C4 C3 C2 120.2(4) . .
C5 C4 C3 120.2(5) . .
C4 C5 C6 120.9(5) . .
C7 C6 C5 119.2(4) . .
C7 C6 N1 121.1(4) . .
C5 C6 N1 119.5(4) . .
C6 C7 C2 120.1(4) . .
O1 C8 N1 127.2(4) . .
O1 C8 C9 121.9(4) . .
N1 C8 C9 110.8(3) . .
N2 C9 C10 120.1(4) . .
N2 C9 C8 112.9(3) . .
C10 C9 C8 127.0(4) . .
C9 C10 C11 117.7(4) . .
C10 C11 C10 121.0(5) . 2
N3 C13 O1W 125(2) . 8_455
O4 C14 N3 49.4(11) . .
C8 N1 C6 120.1(3) . .
C8 N1 Co1 115.9(3) . .
C6 N1 Co1 124.0(3) . .
C9 N2 C9 123.5(5) 2 .
C9 N2 Co1 118.3(2) 2 .
C9 N2 Co1 118.3(2) . .
O4 N3 C13 118.1(18) . .
O4 N3 C12 115.2(14) . .
C13 N3 C12 105.0(14) . .
O4 N3 C14 60.8(13) . .
C13 N3 C14 139.8(14) . .
C12 N3 C14 111.0(9) . .
N3 O4 C14 69.7(14) . .
N2 Co1 N2 180.0 . 7
N2 Co1 N1 81.94(9) . 2
N2 Co1 N1 98.06(9) 7 2
N2 Co1 N1 98.06(9) . 8
N2 Co1 N1 81.94(9) 7 8
N1 Co1 N1 91.13(2) 2 8
N2 Co1 N1 81.94(9) . .
N2 Co1 N1 98.06(9) 7 .
N1 Co1 N1 163.87(17) 2 .
N1 Co1 N1 91.13(2) 8 .
N2 Co1 N1 98.06(9) . 7
N2 Co1 N1 81.94(9) 7 7
N1 Co1 N1 91.13(2) 2 7
N1 Co1 N1 163.87(17) 8 7
N1 Co1 N1 91.13(2) . 7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.185(7) .
C1 O3 1.303(6) .
C1 C2 1.498(7) .
C2 C3 1.385(7) .
C2 C7 1.389(7) .
C3 C4 1.372(8) .
C4 C5 1.363(7) .
C5 C6 1.385(7) .
C6 C7 1.383(6) .
C6 N1 1.440(5) .
C8 O1 1.244(5) .
C8 N1 1.334(5) .
C8 C9 1.504(6) .
C9 N2 1.327(4) .
C9 C10 1.391(6) .
C10 C11 1.393(6) .
C11 C10 1.393(6) 2
C12 N3 1.424(14) .
C13 N3 1.422(17) .
C13 O1W 1.60(3) 8_455
C14 O4 1.45(3) .
C14 N3 1.561(12) .
N1 Co1 1.949(3) .
N2 C9 1.327(4) 2
N2 Co1 1.854(4) .
N3 O4 1.26(2) .
O1W C13 1.60(3) 7_565
Co1 N2 1.854(4) 7
Co1 N1 1.949(3) 2
Co1 N1 1.949(3) 8
Co1 N1 1.949(3) 7
