#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:57:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179163 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/24/4312471.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_4312471
loop_
_publ_author_name
'Chuanjiang Hu'
'Robert M. Chin'
'Thoi D. Nguyen'
'Khoi T. Nguyen'
'Paul S. Wagenknecht'
'Lawrence C. Nathan'
_publ_contact_author_address
;
         Department of Chemistry
         San Jose State University
         San Jose, CA 95192
;
_publ_contact_author_email       pwagen@jupiter.sjsu.edu
_publ_contact_author_fax         408-924-4945
_publ_contact_author_name        'Paul S. Wagenknecht'
_publ_contact_author_phone       408-924-5008
_publ_section_title
;
 Chemistry of Constrained Dioxocyclam Ligands with Co(III): Unusual
 Examples of C-H and C-N Bond Cleavage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7602
_journal_page_last               7607
_journal_paper_doi               10.1021/ic0302027
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C13 H23 Co N4 O3, 3 (H2 O), 2 (H O0.50)'
_chemical_formula_sum            'C13 H31 Co N4 O7'
_chemical_formula_weight         414.35
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           'Siemens SHELXTL v. 5.03 1994'
_cell_angle_alpha                90.00
_cell_angle_beta                 105.115(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.824(2)
_cell_length_b                   9.189(2)
_cell_length_c                   11.3108(13)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    298
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      4.92
_cell_volume                     1788.4(5)
_computing_cell_refinement       'Siemens XSCANS v. 2.2 1995'
_computing_data_collection       'Siemens XSCANS v. 2.2 1995'
_computing_data_reduction        'Siemens XSCANS v. 2.2 1995'
_computing_molecular_graphics    'Siemens SHELXTL v. 5.03 1994'
_computing_publication_material  'Siemens SHELXTL v. 5.03 1994'
_computing_structure_refinement  'Siemens SHELXTL v. 5.03 1994'
_computing_structure_solution    'Siemens SHELXTL v. 5.03 1994'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Siemens Bruker AXS P4'
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2088
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
' S.Parkin,et.al.,J.Appl.Crystallog.,1995,28,53-56'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       pillar
_exptl_crystal_F_000             880.0
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0028(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     ' SHELXL v. 5.03  1994'
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1679
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0618P)²+2.0112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                1466
_reflns_number_total             1679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0302027_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4312471
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Co Co 0.65539(3) 0.5000 0.63319(4) 0.0193(2) Uani 1 d S .
O1 O 0.62616(12) 0.7558(2) 0.3252(2) 0.0308(5) Uani 1 d . .
N1 N 0.64331(14) 0.6529(3) 0.5145(2) 0.0248(5) Uani 1 d . .
N2 N 0.65454(13) 0.6544(3) 0.7506(2) 0.0242(5) Uani 1 d . .
C1 C 0.6403(2) 0.5000 0.3369(4) 0.0267(9) Uani 1 d S .
H1A H 0.6890 0.5000 0.3139 0.032 Uiso 1 calc SR .
H1B H 0.5994 0.5000 0.2611 0.032 Uiso 1 calc SR .
C2 C 0.63560(15) 0.6454(3) 0.3964(2) 0.0225(6) Uani 1 d . .
C3 C 0.6399(2) 0.7999(3) 0.5640(3) 0.0359(7) Uani 1 d . .
H3A H 0.5864 0.8327 0.5467 0.043 Uiso 1 calc R .
H3B H 0.6687 0.8676 0.5268 0.043 Uiso 1 calc R .
C4 C 0.6755(2) 0.7930(3) 0.7018(3) 0.0330(7) Uani 1 d . .
H4A H 0.7316 0.8008 0.7192 0.040 Uiso 1 calc R .
H4B H 0.6567 0.8737 0.7413 0.040 Uiso 1 calc R .
C5 C 0.7013(2) 0.6389(4) 0.8803(2) 0.0331(7) Uani 1 d . .
H5A H 0.6901 0.7208 0.9270 0.040 Uiso 1 calc R .
H5B H 0.7560 0.6435 0.8824 0.040 Uiso 1 calc R .
C6 C 0.6866(3) 0.5000 0.9416(4) 0.0385(11) Uani 1 d S .
H6A H 0.7192 0.5000 1.0250 0.046 Uiso 1 calc SR .
H6B H 0.6330 0.5000 0.9460 0.046 Uiso 1 calc SR .
C7 C 0.5682(2) 0.6405(3) 0.7350(3) 0.0291(7) Uani 1 d . .
H7A H 0.5400 0.7214 0.6890 0.035 Uiso 1 calc R .
H7B H 0.5558 0.6333 0.8133 0.035 Uiso 1 calc R .
C8 C 0.5516(2) 0.5000 0.6640(4) 0.0257(9) Uani 1 d S .
H8 H 0.5069 0.5000 0.5918 0.031 Uiso 1 calc SR .
O2 O 0.7794(2) 0.5000 0.6677(3) 0.0378(8) Uani 1 d S .
H02A H 0.8083 0.5727 0.6643 0.057 Uiso 1 d R .
O3 O 0.5178(2) 1.0000 0.2910(3) 0.0486(9) Uani 1 d S .
H03A H 0.5487 0.9294 0.3156 0.073 Uiso 1 d R .
O4 O 0.3989(2) 1.0000 0.0644(4) 0.0647(12) Uani 1 d S .
H04A H 0.4401 1.0000 0.1227 0.097 Uiso 1 d SR .
H04B H 0.4227 1.0000 0.0084 0.097 Uiso 1 d SR .
O5 O 0.5824(2) 0.7463(4) 0.0667(3) 0.0812(11) Uani 1 d . .
H05A H 0.5458 0.7431 0.1021 0.122 Uiso 1 d R .
H05B H 0.5908 0.8361 0.0577 0.122 Uiso 1 d R .
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
_geom_angle_publ_flag
N1 Co N1 94.33(14) 6_565 . ?
N1 Co N2 173.31(10) 6_565 . ?
N1 Co N2 85.62(10) . . ?
N1 Co N2 85.62(10) 6_565 6_565 ?
N1 Co N2 173.31(10) . 6_565 ?
N2 Co N2 93.65(14) . 6_565 ?
N1 Co C8 100.65(11) 6_565 . ?
N1 Co C8 100.65(11) . . ?
N2 Co C8 72.82(10) . . ?
N2 Co C8 72.82(10) 6_565 . ?
N1 Co O2 92.84(10) 6_565 . ?
N1 Co O2 92.84(9) . . ?
N2 Co O2 93.85(9) . . ?
N2 Co O2 93.85(9) 6_565 . ?
C8 Co O2 160.1(2) . . ?
N1 Co C7 88.53(10) 6_565 6_565 ?
N1 Co C7 136.58(10) . 6_565 ?
N2 Co C7 86.93(10) . 6_565 ?
N2 Co C7 36.73(9) 6_565 6_565 ?
C8 Co C7 36.79(8) . 6_565 ?
O2 Co C7 130.34(10) . 6_565 ?
N1 Co C7 136.58(10) 6_565 . ?
N1 Co C7 88.53(10) . . ?
N2 Co C7 36.73(9) . . ?
N2 Co C7 86.93(10) 6_565 . ?
C8 Co C7 36.79(8) . . ?
O2 Co C7 130.34(10) . . ?
C7 Co C7 61.69(14) 6_565 . ?
C2 N1 C3 115.7(2) . . ?
C2 N1 Co 129.7(2) . . ?
C3 N1 Co 114.6(2) . . ?
C4 N2 C5 108.6(2) . . ?
C4 N2 C7 112.4(2) . . ?
C5 N2 C7 113.4(2) . . ?
C4 N2 Co 109.1(2) . . ?
C5 N2 Co 119.9(2) . . ?
C7 N2 Co 92.7(2) . . ?
C2 C1 C2 124.7(3) . 6_565 ?
C2 C1 H1A 106.1 . . ?
C2 C1 H1A 106.1 6_565 . ?
C2 C1 H1B 106.1 . . ?
C2 C1 H1B 106.1 6_565 . ?
H1A C1 H1B 106.3 . . ?
O1 C2 N1 124.2(3) . . ?
O1 C2 C1 115.8(2) . . ?
N1 C2 C1 119.9(3) . . ?
N1 C3 C4 107.7(2) . . ?
N1 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 . . ?
N1 C3 H3B 110.2 . . ?
C4 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
N2 C4 C3 109.9(2) . . ?
N2 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
N2 C4 H4B 109.68 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 114.4(3) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 C5 115.6(4) 6_565 . ?
C5 C6 H6A 108.4 6_565 . ?
C5 C6 H6A 108.4 . . ?
C5 C6 H6B 108.4 6_565 . ?
C5 C6 H6B 108.4 . . ?
H6A C6 H6B 107.4 . . ?
N2 C7 C8 100.9(2) . . ?
N2 C7 Co 50.55(12) . . ?
C8 C7 Co 51.5(2) . . ?
N2 C7 H7A 111.60 . . ?
C8 C7 H7A 111.6 . . ?
Co C7 H7A 116.33 . . ?
N2 C7 H7B 111.60 . . ?
C8 C7 H7B 111.6 . . ?
Co C7 H7B 134.28 . . ?
H7A C7 H7B 109.4 . . ?
C7 C8 C7 117.7(3) . 6_565 ?
C7 C8 Co 91.7(2) . . ?
C7 C8 Co 91.7(2) 6_565 . ?
C7 C8 H8 116.6 . . ?
C7 C8 H8 116.6 6_565 . ?
Co C8 H8 116.62 . . ?
Co O2 H02A 126.84 . . ?
H04A O4 H04B 94.5 . . ?
H05A O5 H05B 105.5 . . ?
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 N1 1.916(2) 6_565 ?
Co N1 1.916(2) . ?
Co N2 1.946(2) . ?
Co N2 1.946(2) 6_565 ?
Co C8 1.970(4) . ?
Co O2 2.143(3) . ?
Co C7 2.517(3) 6_565 ?
Co C7 2.517(3) . ?
O1 C2 1.279(3) . ?
N1 C2 1.309(3) . ?
N1 C3 1.470(4) . ?
N2 C4 1.474(4) . ?
N2 C5 1.493(3) . ?
N2 C7 1.507(4) . ?
C1 C2 1.508(3) . ?
C1 C2 1.508(3) 6_565 ?
C1 H1A 0.97 . ?
C1 H1B 0.97 . ?
C3 C4 1.523(5) . ?
C3 H3A 0.97 . ?
C3 H3B 0.97 . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C5 C6 1.508(4) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C6 C5 1.508(4) 6_565 ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C7 C8 1.508(3) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C8 C7 1.508(3) 6_565 ?
C8 H8 0.98 . ?
O2 H02A 0.85 . ?
O3 H03A 0.85 . ?
O4 H04A 0.85 . ?
O4 H04B 0.85 . ?
O5 H05A 0.85 . ?
O5 H05B 0.85 . ?
