#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:29:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179143 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/04/4310472.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_4310472
loop_
_publ_author_name
'Kaian Yao'
'Xin Zhang'
'Huilan Chen'
'Yuhua Mei'
'Yizhi Li'
_publ_section_title
;
 Synthesis and Crystal Structures of A New Series of Intramolecular
 Bridged Alkylcobaloxime Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              577
_journal_page_last               583
_journal_paper_doi               10.1021/ic035147g
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'Cl O4, C16 H25 Co N5 O4'
_chemical_formula_sum            'C16 H25 Cl Co N5 O8'
_chemical_formula_weight         509.79
_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                 95.71(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.315(1)
_cell_length_b                   11.812(1)
_cell_length_c                   22.357(2)
_cell_measurement_reflns_used    3496
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      2.46
_cell_volume                     2184.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10922
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0526
_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)+(0.0884P)²+0.5191P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                2966
_reflns_number_total             3839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035147gsi20031003_094513_3.cif
_cod_data_source_block           for_compound4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4310472
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
Co1 Co 0.32513(5) 0.74241(4) 0.40817(2) 0.03804(19) Uani 1 1 d . . .
C1 C 0.4243(5) 0.6098(4) 0.24285(18) 0.0607(11) Uani 1 1 d . . .
H1A H 0.5054 0.5518 0.2478 0.091 Uiso 1 1 calc R . .
H1B H 0.4506 0.6620 0.2124 0.091 Uiso 1 1 calc R . .
H1C H 0.3210 0.5760 0.2311 0.091 Uiso 1 1 calc R . .
C2 C 0.4180(4) 0.6709(3) 0.30036(15) 0.0423(8) Uani 1 1 d . . .
C3 C 0.5475(5) 0.7444(3) 0.32587(18) 0.0449(9) Uani 1 1 d . . .
C4 C 0.6882(5) 0.7776(4) 0.2943(2) 0.0612(11) Uani 1 1 d . . .
H4A H 0.7362 0.8448 0.3125 0.092 Uiso 1 1 calc R . .
H4B H 0.6536 0.7921 0.2528 0.092 Uiso 1 1 calc R . .
H4C H 0.7663 0.7175 0.2973 0.092 Uiso 1 1 calc R . .
C5 C 0.2519(7) 0.8823(4) 0.5751(2) 0.0820(16) Uani 1 1 d . . .
H5A H 0.3455 0.8574 0.6002 0.123 Uiso 1 1 calc R . .
H5B H 0.1565 0.8658 0.5944 0.123 Uiso 1 1 calc R . .
H5C H 0.2588 0.9625 0.5686 0.123 Uiso 1 1 calc R . .
C6 C 0.2437(5) 0.8221(3) 0.51597(16) 0.0515(10) Uani 1 1 d . . .
C7 C 0.0979(5) 0.7659(3) 0.48830(17) 0.0478(9) Uani 1 1 d . . .
C8 C -0.0576(6) 0.7636(5) 0.5162(2) 0.0780(15) Uani 1 1 d . . .
H8A H -0.1054 0.8376 0.5140 0.117 Uiso 1 1 calc R . .
H8B H -0.0375 0.7411 0.5575 0.117 Uiso 1 1 calc R . .
H8C H -0.1299 0.7105 0.4951 0.117 Uiso 1 1 calc R . .
C9 C 0.2567(6) 0.4739(4) 0.3576(2) 0.0752(14) Uani 1 1 d . . .
H9A H 0.1820 0.4112 0.3504 0.090 Uiso 1 1 calc R . .
H9B H 0.3578 0.4527 0.3424 0.090 Uiso 1 1 calc R . .
C10 C 0.2862(6) 0.4959(3) 0.4252(2) 0.0601(11) Uani 1 1 d . . .
H10A H 0.1832 0.5120 0.4403 0.072 Uiso 1 1 calc R . .
H10B H 0.3285 0.4273 0.4447 0.072 Uiso 1 1 calc R . .
C11 C 0.4017(5) 0.5925(3) 0.44313(18) 0.0523(10) Uani 1 1 d . . .
H11A H 0.5065 0.5752 0.4299 0.063 Uiso 1 1 calc R . .
H11B H 0.4150 0.5984 0.4866 0.063 Uiso 1 1 calc R . .
C12 C 0.2972(5) 0.9948(3) 0.38818(19) 0.0519(10) Uani 1 1 d . . .
H12 H 0.3819 0.9963 0.4187 0.062 Uiso 1 1 calc R . .
C13 C 0.2398(6) 1.0950(4) 0.3652(2) 0.0653(12) Uani 1 1 d . . .
H13 H 0.2856 1.1631 0.3790 0.078 Uiso 1 1 calc R . .
C14 C 0.1118(6) 1.0937(4) 0.3206(2) 0.0702(13) Uani 1 1 d . . .
H14 H 0.0679 1.1608 0.3045 0.084 Uiso 1 1 calc R . .
C15 C 0.0516(6) 0.9916(4) 0.3009(2) 0.0686(12) Uani 1 1 d . . .
H15 H -0.0338 0.9880 0.2708 0.082 Uiso 1 1 calc R . .
C16 C 0.1177(5) 0.8947(4) 0.32579(18) 0.0564(10) Uani 1 1 d . . .
H16 H 0.0761 0.8256 0.3115 0.068 Uiso 1 1 calc R . .
H3 H 0.578(6) 0.852(4) 0.464(3) 0.099(16) Uiso 1 1 d . . .
N1 N 0.3041(3) 0.6634(2) 0.33539(13) 0.0423(7) Uani 1 1 d . . .
N2 N 0.5260(4) 0.7758(2) 0.38003(14) 0.0431(7) Uani 1 1 d . . .
N3 N 0.3622(4) 0.8137(3) 0.48381(13) 0.0464(7) Uani 1 1 d . . .
N4 N 0.1213(4) 0.7195(2) 0.43811(13) 0.0428(7) Uani 1 1 d . . .
N5 N 0.2385(4) 0.8940(2) 0.36939(13) 0.0424(7) Uani 1 1 d . . .
O1 O 0.1873(3) 0.5784(3) 0.32329(14) 0.0649(8) Uani 1 1 d . . .
O2 O 0.6363(3) 0.8403(2) 0.41086(13) 0.0581(7) Uani 1 1 d . . .
O3 O 0.5071(4) 0.8582(3) 0.50453(13) 0.0642(8) Uani 1 1 d . . .
O4 O -0.0143(3) 0.6692(3) 0.40830(14) 0.0781(10) Uani 1 1 d . . .
H4 H 0.0326 0.6243 0.3905 0.094 Uiso 1 1 d R . .
Cl1 Cl 0.23814(15) 0.90325(9) 0.15834(6) 0.0690(3) Uani 1 1 d . . .
O6 O 0.3710(6) 0.8759(5) 0.1962(4) 0.190(3) Uani 1 1 d . A 1
O7 O 0.1149(5) 0.8296(3) 0.1705(2) 0.1143(14) Uani 1 1 d . A 1
O8 O 0.3040(19) 0.889(2) 0.1029(11) 0.160(8) Uani 0.60 1 d P A 1
O9 O 0.1991(6) 1.0164(3) 0.1710(2) 0.1142(14) Uani 1 1 d . A 1
O8' O 0.213(3) 0.897(4) 0.0954(18) 0.160(8) Uani 0.40 1 d P A 2
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
N1 Co1 N2 79.79(13) . . ?
N1 Co1 N3 174.88(13) . . ?
N2 Co1 N3 97.73(13) . . ?
N1 Co1 N4 103.08(13) . . ?
N2 Co1 N4 175.99(12) . . ?
N3 Co1 N4 79.63(13) . . ?
N1 Co1 C11 84.11(14) . . ?
N2 Co1 C11 93.27(15) . . ?
N3 Co1 C11 91.59(15) . . ?
N4 Co1 C11 89.82(15) . . ?
N1 Co1 N5 93.90(12) . . ?
N2 Co1 N5 87.87(12) . . ?
N3 Co1 N5 90.47(12) . . ?
N4 Co1 N5 89.14(12) . . ?
C11 Co1 N5 177.49(13) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 111.2(3) . . ?
N1 C2 C1 125.9(3) . . ?
C3 C2 C1 122.9(3) . . ?
N2 C3 C2 111.8(3) . . ?
N2 C3 C4 124.0(4) . . ?
C2 C3 C4 124.2(4) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 C7 112.3(3) . . ?
N3 C6 C5 124.2(4) . . ?
C7 C6 C5 123.5(4) . . ?
N4 C7 C6 111.8(4) . . ?
N4 C7 C8 124.9(4) . . ?
C6 C7 C8 123.2(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 O1 111.9(4) . . ?
C10 C9 H9A 109.2 . . ?
O1 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
O1 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C11 C10 C9 115.1(4) . . ?
C11 C10 H10A 108.5 . . ?
C9 C10 H10A 108.5 . . ?
C11 C10 H10B 108.5 . . ?
C9 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
C10 C11 Co1 113.0(3) . . ?
C10 C11 H11A 109.0 . . ?
Co1 C11 H11A 109.0 . . ?
C10 C11 H11B 109.0 . . ?
Co1 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N5 C12 C13 123.6(4) . . ?
N5 C12 H12 118.2 . . ?
C13 C12 H12 118.2 . . ?
C12 C13 C14 118.6(4) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
C15 C14 C13 118.3(4) . . ?
C15 C14 H14 120.8 . . ?
C13 C14 H14 120.8 . . ?
C14 C15 C16 119.4(4) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
N5 C16 C15 123.3(4) . . ?
N5 C16 H16 118.4 . . ?
C15 C16 H16 118.4 . . ?
C2 N1 O1 117.8(3) . . ?
C2 N1 Co1 118.9(2) . . ?
O1 N1 Co1 121.8(2) . . ?
C3 N2 O2 119.7(3) . . ?
C3 N2 Co1 117.5(3) . . ?
O2 N2 Co1 122.3(2) . . ?
C6 N3 O3 119.1(3) . . ?
C6 N3 Co1 118.1(3) . . ?
O3 N3 Co1 122.7(2) . . ?
C7 N4 O4 114.7(3) . . ?
C7 N4 Co1 117.8(3) . . ?
O4 N4 Co1 127.1(2) . . ?
C16 N5 C12 116.8(3) . . ?
C16 N5 Co1 121.0(3) . . ?
C12 N5 Co1 122.2(3) . . ?
N1 O1 C9 105.1(3) . . ?
N2 O2 H3 103(2) . . ?
N3 O3 H3 103(3) . . ?
N4 O4 H4 96.4 . . ?
O6 Cl1 O7 107.3(3) . . ?
O6 Cl1 O8' 129.9(14) . . ?
O7 Cl1 O8' 97.0(11) . . ?
O6 Cl1 O9 106.8(3) . . ?
O7 Cl1 O9 111.4(3) . . ?
O8' Cl1 O9 103.8(19) . . ?
O6 Cl1 O8 99.0(11) . . ?
O7 Cl1 O8 117.1(8) . . ?
O8' Cl1 O8 31.5(18) . . ?
O9 Cl1 O8 113.9(12) . . ?
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
Co1 N1 1.868(3) . ?
Co1 N2 1.884(3) . ?
Co1 N3 1.887(3) . ?
Co1 N4 1.903(3) . ?
Co1 C11 2.013(4) . ?
Co1 N5 2.086(3) . ?
C1 C2 1.480(5) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.290(4) . ?
C2 C3 1.455(5) . ?
C3 N2 1.296(5) . ?
C3 C4 1.478(5) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.498(6) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N3 1.280(5) . ?
C6 C7 1.464(5) . ?
C7 N4 1.281(5) . ?
C7 C8 1.490(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.529(6) . ?
C9 O1 1.534(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.519(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N5 1.339(5) . ?
C12 C13 1.359(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.384(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.361(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.364(6) . ?
C15 H15 0.9300 . ?
C16 N5 1.328(5) . ?
C16 H16 0.9300 . ?
N1 O1 1.405(4) . ?
N2 O2 1.331(4) . ?
N3 O3 1.353(4) . ?
N4 O4 1.385(4) . ?
O2 H3 1.33(6) . ?
O3 H3 1.13(6) . ?
O4 H4 0.7892 . ?
Cl1 O6 1.362(5) . ?
Cl1 O7 1.391(4) . ?
Cl1 O8' 1.40(4) . ?
Cl1 O9 1.411(4) . ?
Cl1 O8 1.414(18) . ?
