#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:02:04 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179552 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/21/4502125.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_4502125
loop_
_publ_author_name
'Adarsh, N. N.'
'Sahoo, Pathik'
'Dastidar, Parthasarathi'
_publ_section_title
;
 Is a Crystal Engineering Approach Useful in Designing Metallogels? A Case
 Study
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4976
_journal_paper_doi               10.1021/cg101078f
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C17 H15 Co N2 O7, H2 O'
_chemical_formula_sum            'C17 H17 Co N2 O8'
_chemical_formula_weight         436.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.000(5)
_cell_angle_beta                 96.824(6)
_cell_angle_gamma                102.660(6)
_cell_formula_units_Z            2
_cell_length_a                   6.344(3)
_cell_length_b                   9.287(4)
_cell_length_c                   16.008(8)
_cell_measurement_temperature    100(2)
_cell_volume                     897.3(7)
_computing_cell_refinement       'BRUKER APEX II'
_computing_data_collection       'BRUKER APEX II'
_computing_data_reduction        'BRUKER APEX II'
_computing_molecular_graphics    'MERCURY 2.3, PLATON-97'
_computing_publication_material  shelxtl-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER CCD AREA DETECTOR'
_diffrn_measurement_method       'PHI-OMEGA SCAN'
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8578
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.8974
_exptl_absorpt_correction_T_min  0.7942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3152
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0485P)²+0.4906P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                2692
_reflns_number_total             3152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101078f_si_002.cif
_cod_data_source_block           7
_cod_original_cell_volume        897.4(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4502125
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Co1 Co 0.93480(6) 0.66252(4) 0.69055(2) 0.01685(14) Uani 1 1 d .
N1 N 0.8050(3) 0.8572(2) 0.72703(13) 0.0177(5) Uani 1 1 d .
C2 C 0.8908(5) 0.9858(3) 0.7022(2) 0.0311(7) Uani 1 1 d .
H2 H 1.0043 0.9881 0.6703 0.037 Uiso 1 1 calc R
C3 C 0.8190(6) 1.1143(4) 0.7218(2) 0.0404(9) Uani 1 1 d .
H3 H 0.8835 1.2010 0.7031 0.048 Uiso 1 1 calc R
C4 C 0.6505(5) 1.1145(3) 0.7692(2) 0.0345(8) Uani 1 1 d .
H4 H 0.5991 1.2004 0.7825 0.041 Uiso 1 1 calc R
C5 C 0.5602(4) 0.9831(3) 0.79629(17) 0.0186(6) Uani 1 1 d .
C6 C 0.6411(4) 0.8577(3) 0.77309(16) 0.0184(6) Uani 1 1 d .
H6 H 0.5785 0.7691 0.7904 0.022 Uiso 1 1 calc R
N7 N 0.3921(3) 0.9691(2) 0.84710(14) 0.0181(5) Uani 1 1 d .
H7 H 0.3322 0.8795 0.8529 0.022 Uiso 1 1 calc R
C8 C 0.3142(4) 1.0816(3) 0.88795(17) 0.0194(6) Uani 1 1 d .
O9 O 0.3719(3) 1.2135(2) 0.88107(13) 0.0275(5) Uani 1 1 d .
C10 C 0.1521(4) 1.0356(3) 0.94532(17) 0.0181(6) Uani 1 1 d .
C11 C -0.0020(4) 1.1203(3) 0.95803(17) 0.0205(6) Uani 1 1 d .
H11 H -0.0031 1.2013 0.9305 0.025 Uiso 1 1 calc R
C12 C 0.1536(4) 0.9165(3) 0.98828(17) 0.0197(6) Uani 1 1 d .
H12 H 0.2576 0.8609 0.9809 0.024 Uiso 1 1 calc R
O13 O 1.1273(3) 0.6737(2) 0.81411(11) 0.0195(4) Uani 1 1 d .
O14 O 0.7813(3) 0.5541(2) 0.78595(12) 0.0217(4) Uani 1 1 d .
C15 C 0.9622(4) 0.5925(3) 0.83595(17) 0.0178(6) Uani 1 1 d .
C16 C 0.9812(4) 0.5426(3) 0.92042(16) 0.0173(6) Uani 1 1 d .
C17 C 0.7943(4) 0.4880(3) 0.95409(17) 0.0190(6) Uani 1 1 d .
H17 H 0.6568 0.4794 0.9233 0.023 Uiso 1 1 calc R
C18 C 0.8124(4) 0.4465(3) 1.03341(17) 0.0195(6) Uani 1 1 d .
H18 H 0.6870 0.4111 1.0562 0.023 Uiso 1 1 calc R
O19 O 1.1442(3) 0.7881(2) 0.62613(13) 0.0260(5) Uani 1 1 d .
O20 O 1.2919(3) 0.6254(2) 0.54934(11) 0.0197(4) Uani 1 1 d .
C21 C 1.2648(4) 0.7559(3) 0.57225(17) 0.0194(6) Uani 1 1 d .
C22 C 1.3850(4) 0.8819(3) 0.53413(18) 0.0216(6) Uani 1 1 d .
C23 C 1.5348(6) 0.8593(4) 0.4814(2) 0.0439(10) Uani 1 1 d .
H23 H 1.5604 0.7641 0.4681 0.053 Uiso 1 1 calc R
C24 C 1.6478(6) 0.9754(4) 0.4480(3) 0.0518(11) Uani 1 1 d .
H24 H 1.7486 0.9570 0.4125 0.062 Uiso 1 1 calc R
O25 O 0.6857(3) 0.5667(2) 0.59343(13) 0.0318(5) Uani 1 1 d D
O26 O 1.0506(3) 0.4680(2) 0.64829(13) 0.0226(4) Uani 1 1 d D
O27 O 0.3448(4) 0.3823(3) 0.7517(2) 0.0576(8) Uani 1 1 d D
H25A H 0.701(6) 0.496(3) 0.5537(16) 0.050(11) Uiso 1 1 d D
H25B H 0.566(4) 0.595(4) 0.580(2) 0.053(11) Uiso 1 1 d D
H26A H 1.134(6) 0.499(5) 0.611(2) 0.072(14) Uiso 1 1 d D
H26B H 1.145(5) 0.439(4) 0.685(2) 0.064(13) Uiso 1 1 d D
H27A H 0.321(7) 0.330(4) 0.793(2) 0.076(15) Uiso 1 1 d D
H27B H 0.478(4) 0.440(5) 0.755(4) 0.12(2) Uiso 1 1 d 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
O25 Co1 O19 99.43(10) . .
O25 Co1 O26 83.49(8) . .
O19 Co1 O26 90.86(8) . .
O25 Co1 O14 95.29(9) . 1
O19 Co1 O14 165.28(8) . 1
O26 Co1 O14 90.49(8) . 1
O25 Co1 O14 95.29(9) . .
O19 Co1 O14 165.28(8) . .
O26 Co1 O14 90.49(8) . .
O25 Co1 O13 153.55(9) . .
O19 Co1 O13 104.88(8) . .
O26 Co1 O13 85.87(7) . .
O14 Co1 O13 60.60(7) 1 .
O14 Co1 O13 60.60(7) . .
O25 Co1 N1 93.53(9) . .
O19 Co1 N1 88.86(8) . .
O26 Co1 N1 176.92(8) . .
O14 Co1 N1 90.55(8) 1 .
O14 Co1 N1 90.55(8) . .
O13 Co1 N1 97.16(8) . .
O25 Co1 C15 124.53(10) . .
O19 Co1 C15 135.28(9) . .
O26 Co1 C15 86.78(8) . .
O14 Co1 C15 30.25(8) 1 .
O14 Co1 C15 30.25(8) . .
O13 Co1 C15 30.39(8) . .
N1 Co1 C15 95.57(8) . .
C2 N1 C6 117.0(2) . .
C2 N1 Co1 118.84(18) . .
C6 N1 Co1 124.17(17) . .
N1 C2 C3 123.1(3) . .
N1 C2 H2 118.5 . .
C3 C2 H2 118.5 . .
C2 C3 C4 119.9(3) . .
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
C3 C4 C5 118.2(3) . .
C3 C4 H4 120.9 . .
C5 C4 H4 120.9 . .
C4 C5 C6 118.3(2) . .
C4 C5 N7 124.0(2) . .
C6 C5 N7 117.7(2) . .
N1 C6 C5 123.6(2) . .
N1 C6 H6 118.2 . .
C5 C6 H6 118.2 . .
C8 N7 C5 127.3(2) . .
C8 N7 H7 116.3 . .
C5 N7 H7 116.3 . .
O9 C8 N7 124.0(2) . .
O9 C8 C10 120.4(2) . .
N7 C8 C10 115.6(2) . .
C12 C10 C11 119.2(2) . .
C12 C10 C8 123.0(2) . .
C11 C10 C8 117.8(2) . .
C12 C11 C10 119.9(3) 2_577 .
C12 C11 H11 120.0 2_577 .
C10 C11 H11 120.0 . .
C11 C12 C10 120.9(3) 2_577 .
C11 C12 H12 119.6 2_577 .
C10 C12 H12 119.6 . .
C15 O13 Co1 89.64(15) . .
C15 O14 Co1 90.01(15) . .
O14 C15 O13 119.6(2) 1 .
O14 C15 O13 119.6(2) . .
O14 C15 C16 120.1(2) 1 .
O14 C15 C16 120.1(2) . .
O13 C15 C16 120.3(2) . .
O14 C15 Co1 59.74(13) 1 .
O14 C15 Co1 59.74(13) . .
O13 C15 Co1 59.97(13) . .
C16 C15 Co1 176.76(18) . .
C17 C16 C18 119.7(2) . 2_767
C17 C16 C15 120.1(2) . .
C18 C16 C15 120.1(2) 2_767 .
C18 C17 C16 120.0(3) . .
C18 C17 H17 120.0 . .
C16 C17 H17 120.0 . .
C17 C18 C16 120.2(3) . 2_767
C17 C18 H18 119.9 . .
C16 C18 H18 119.9 2_767 .
C21 O19 Co1 133.60(18) . .
O19 C21 O20 124.1(2) . 1
O19 C21 O20 124.1(2) . .
O19 C21 C22 117.4(2) . .
O20 C21 C22 118.5(2) 1 .
O20 C21 C22 118.5(2) . .
C23 C22 C24 117.5(3) . 2_876
C23 C22 C21 121.0(3) . .
C24 C22 C21 121.5(3) 2_876 .
C22 C23 C24 121.0(3) . .
C22 C23 H23 119.5 . .
C24 C23 H23 119.5 . .
C23 C24 C22 121.6(3) . 2_876
C23 C24 H24 119.2 . .
C22 C24 H24 119.2 2_876 .
Co1 O25 H25A 119(2) . .
Co1 O25 H25B 129(2) . .
H25A O25 H25B 111(3) . .
Co1 O26 H26A 102(3) . .
Co1 O26 H26B 120(3) . .
H26A O26 H26B 101(4) . .
H27A O27 H27B 118(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O25 2.018(2) .
Co1 O19 2.052(2) .
Co1 O26 2.140(2) .
Co1 O14 2.1678(19) 1
Co1 O14 2.1678(19) .
Co1 O13 2.173(2) .
Co1 N1 2.174(2) .
Co1 C15 2.510(3) .
N1 C2 1.339(4) .
N1 C6 1.344(3) .
C2 C3 1.373(4) .
C2 H2 0.9300 .
C3 C4 1.383(4) .
C3 H3 0.9300 .
C4 C5 1.388(4) .
C4 H4 0.9300 .
C5 C6 1.389(4) .
C5 N7 1.412(3) .
C6 H6 0.9300 .
N7 C8 1.361(3) .
N7 H7 0.8600 .
C8 O9 1.226(3) .
C8 C10 1.496(4) .
C10 C12 1.392(4) .
C10 C11 1.397(4) .
C11 C12 1.387(4) 2_577
C11 H11 0.9300 .
C12 C11 1.387(4) 2_577
C12 H12 0.9300 .
O13 C15 1.270(3) .
O14 O14 0.000(6) 1
O14 C15 1.264(3) .
C15 O14 1.264(3) 1
C15 C16 1.496(4) .
C16 C17 1.389(4) .
C16 C18 1.400(4) 2_767
C17 C18 1.383(4) .
C17 H17 0.9300 .
C18 C16 1.400(4) 2_767
C18 H18 0.9300 .
O19 C21 1.263(3) .
O20 O20 0.000(6) 1
O20 C21 1.265(3) .
C21 O20 1.265(3) 1
C21 C22 1.505(4) .
C22 C23 1.372(4) .
C22 C24 1.378(4) 2_876
C23 C24 1.377(4) .
C23 H23 0.9300 .
C24 C22 1.378(4) 2_876
C24 H24 0.9300 .
O25 H25A 0.869(10) .
O25 H25B 0.870(10) .
O26 H26A 0.881(10) .
O26 H26B 0.898(10) .
O27 H27A 0.889(10) .
O27 H27B 0.886(11) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7 O13 0.86 2.02 2.818(3) 154.3 1_455
O25 H25A O20 0.869(10) 1.859(13) 2.709(3) 166(3) 2_766
O25 H25B O20 0.870(10) 1.844(12) 2.708(3) 172(4) 1_455
O26 H26A O20 0.881(10) 1.857(18) 2.703(3) 160(4) 1
O26 H26B O27 0.898(10) 1.784(11) 2.681(3) 176(4) 1_655
O27 H27A O9 0.889(10) 1.944(18) 2.797(3) 161(4) 1_545
O27 H27B O14 0.886(11) 1.948(17) 2.818(3) 167(5) 1
