#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:43:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179421 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/18/4331861.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4331861
loop_
_publ_author_name
'Telfer, Shane G.'
'Kuroda, Reiko'
'Lefebvre, Julie'
'Leznoff, Daniel B.'
_publ_section_title
;
 Boxes, Helicates, and Coordination Polymers:  A Structural and
 Magnetochemical Investigation of the Diverse Coordination Chemistry of
 Simple Pyridine-Alcohol Ligands
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4592
_journal_page_last               4601
_journal_paper_doi               10.1021/ic0517218
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C21 H24 Co2 N4 O6'
_chemical_formula_weight         546.30
_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                110.938(2)
_cell_angle_beta                 91.528(3)
_cell_angle_gamma                107.942(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3991(15)
_cell_length_b                   11.4750(18)
_cell_length_c                   11.9191(19)
_cell_measurement_temperature    110(2)
_cell_volume                     1128.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'Bruker APEX'
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6824
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.515
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8046
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red-pink
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.311
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0665
_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)+(0.0308P)²+17.9184P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2101
_refine_ls_wR_factor_ref         0.2116
_reflns_number_gt                4109
_reflns_number_total             4813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0517218sup1.cif
_cod_data_source_block           Figure_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4331861
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 0.36824(10) 0.64499(9) 0.65823(8) 0.0126(2) Uani 1 1 d .
Co2 Co 0.57006(10) 0.62722(9) 0.45715(8) 0.0128(2) Uani 1 1 d .
C13 C 0.0480(8) 0.9944(7) 0.6596(7) 0.0209(15) Uani 1 1 d .
H13 H 0.1389 1.0564 0.7067 0.025 Uiso 1 1 calc R
C14 C 0.2435(9) 0.6341(7) 0.2024(7) 0.0206(15) Uani 1 1 d .
H14 H 0.1434 0.6295 0.2076 0.025 Uiso 1 1 calc R
C15 C 0.5393(9) 0.6465(7) 0.1934(6) 0.0187(14) Uani 1 1 d .
C16 C 0.4080(9) 0.9728(7) 0.8034(7) 0.0235(16) Uani 1 1 d .
H16A H 0.3850 0.9500 0.7177 0.035 Uiso 1 1 calc R
H16B H 0.4226 1.0651 0.8464 0.035 Uiso 1 1 calc R
H16C H 0.3256 0.9201 0.8296 0.035 Uiso 1 1 calc R
C17 C 0.7875(8) 0.9374(7) 0.5804(6) 0.0172(14) Uani 1 1 d .
C18 C 0.4520(9) 0.6376(7) 0.0933(7) 0.0226(16) Uani 1 1 d .
H18 H 0.4945 0.6372 0.0236 0.027 Uiso 1 1 calc R
C19 C 0.6519(8) 0.9742(7) 0.5601(7) 0.0212(15) Uani 1 1 d .
H19A H 0.6472 0.9828 0.4830 0.032 Uiso 1 1 calc R
H19B H 0.6599 1.0570 0.6237 0.032 Uiso 1 1 calc R
H19C H 0.5618 0.9063 0.5607 0.032 Uiso 1 1 calc R
C20 C 0.8098(9) 0.8929(7) 0.8654(7) 0.0217(15) Uani 1 1 d .
H20 H 0.8968 0.8730 0.8756 0.026 Uiso 1 1 calc R
C21 C 0.0366(8) 0.8644(7) 0.6000(7) 0.0199(15) Uani 1 1 d .
H21 H 0.1192 0.8373 0.6056 0.024 Uiso 1 1 calc R
C22 C 0.1155(8) 0.3692(6) 0.5453(7) 0.0167(14) Uani 1 1 d .
H22A H 0.0692 0.4036 0.4965 0.020 Uiso 1 1 calc R
H22B H 0.0620 0.3715 0.6141 0.020 Uiso 1 1 calc R
C23 C -0.1018(8) 0.7735(7) 0.5306(6) 0.0167(14) Uani 1 1 d .
C24 C 0.3364(8) 0.6461(7) 0.3018(6) 0.0167(14) Uani 1 1 d .
C25 C 0.6757(8) 0.6547(7) 0.7211(6) 0.0168(14) Uani 1 1 d .
H25A H 0.7717 0.6566 0.6924 0.020 Uiso 1 1 calc R
H25B H 0.6619 0.6081 0.7760 0.020 Uiso 1 1 calc R
C26 C 0.7006(9) 0.6496(7) 0.1919(7) 0.0217(15) Uani 1 1 d .
H26A H 0.7630 0.7192 0.2645 0.033 Uiso 1 1 calc R
H26B H 0.7360 0.6656 0.1221 0.033 Uiso 1 1 calc R
H26C H 0.7056 0.5660 0.1880 0.033 Uiso 1 1 calc R
C27 C 0.8064(10) 1.0203(8) 0.9258(7) 0.0268(17) Uani 1 1 d .
H27 H 0.8914 1.0869 0.9779 0.032 Uiso 1 1 calc R
C28 C -0.0761(9) 1.0336(7) 0.6498(7) 0.0214(15) Uani 1 1 d .
H28 H -0.0688 1.1219 0.6884 0.026 Uiso 1 1 calc R
C29 C 0.5502(9) 0.9466(7) 0.8295(6) 0.0197(15) Uani 1 1 d .
C30 C 0.6795(8) 0.7957(7) 0.7892(6) 0.0173(14) Uani 1 1 d .
C31 C 0.3016(10) 0.6291(8) 0.0959(7) 0.0259(17) Uani 1 1 d .
H31 H 0.2416 0.6204 0.0281 0.031 Uiso 1 1 calc R
C32 C 0.6764(9) 1.0473(8) 0.9082(7) 0.0256(17) Uani 1 1 d .
H32 H 0.6729 1.1320 0.9484 0.031 Uiso 1 1 calc R
C33 C 0.2784(8) 0.6540(7) 0.4198(6) 0.0170(14) Uani 1 1 d .
H33A H 0.2257 0.7176 0.4414 0.020 Uiso 1 1 calc R
H33B H 0.2066 0.5681 0.4095 0.020 Uiso 1 1 calc R
N9 N 0.7746(7) 0.8078(6) 0.5248(5) 0.0167(12) Uani 1 1 d .
N10 N 0.1575(7) 0.6633(6) 0.7941(6) 0.0195(13) Uani 1 1 d .
N11 N 0.4808(7) 0.6496(5) 0.2982(5) 0.0153(12) Uani 1 1 d .
N12 N 0.5521(7) 0.8218(6) 0.7729(5) 0.0154(12) Uani 1 1 d .
O3 O 0.1474(6) 0.6671(5) 0.6905(5) 0.0218(11) Uani 1 1 d .
O4 O 0.2809(6) 0.6572(5) 0.8337(5) 0.0199(11) Uani 1 1 d .
O5 O 0.5580(5) 0.5863(5) 0.6217(4) 0.0161(10) Uani 1 1 d .
O6 O 0.3967(5) 0.6921(5) 0.5145(4) 0.0155(10) Uani 1 1 d .
O7 O 0.2679(5) 0.4491(5) 0.5872(5) 0.0166(10) Uani 1 1 d .
O8 O 0.0555(7) 0.6663(6) 0.8571(6) 0.0369(15) Uani 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
O6 Co1 O7 103.6(2) . .
O6 Co1 O5 84.8(2) . .
O7 Co1 O5 80.1(2) . .
O6 Co1 N12 92.5(2) . .
O7 Co1 N12 151.2(2) . .
O5 Co1 N12 77.8(2) . .
O6 Co1 O3 100.2(2) . .
O7 Co1 O3 89.4(2) . .
O5 Co1 O3 169.2(2) . .
N12 Co1 O3 111.3(2) . .
O6 Co1 O4 153.9(2) . .
O7 Co1 O4 91.0(2) . .
O5 Co1 O4 119.32(19) . .
N12 Co1 O4 84.0(2) . .
O3 Co1 O4 57.93(19) . .
O7 Co2 O6 173.2(2) 2_666 .
O7 Co2 O5 92.2(2) 2_666 .
O6 Co2 O5 81.58(19) . .
O7 Co2 N11 108.0(2) 2_666 .
O6 Co2 N11 77.5(2) . .
O5 Co2 N11 155.6(2) . .
O7 Co2 O5 78.02(19) 2_666 2_666
O6 Co2 O5 98.14(19) . 2_666
O5 Co2 O5 80.26(19) . 2_666
N11 Co2 O5 90.4(2) . 2_666
O7 Co2 N9 78.5(2) 2_666 .
O6 Co2 N9 104.9(2) . .
O5 Co2 N9 98.1(2) . .
N11 Co2 N9 99.3(2) . .
O5 Co2 N9 156.4(2) 2_666 .
C21 C13 C28 120.0(7) . .
C31 C14 C24 119.3(7) . .
N11 C15 C18 121.1(7) . .
N11 C15 C26 116.8(6) . .
C18 C15 C26 122.0(7) . .
N9 C17 C28 121.3(7) . 1_655
N9 C17 C19 117.3(6) . .
C28 C17 C19 121.4(6) 1_655 .
C15 C18 C31 120.6(7) . .
C27 C20 C30 118.3(7) . .
C13 C21 C23 118.6(7) . .
O7 C22 C23 110.7(6) . 2_566
N9 C23 C21 122.3(6) 1_455 .
N9 C23 C22 117.5(6) 1_455 2_566
C21 C23 C22 120.2(6) . 2_566
N11 C24 C14 122.8(7) . .
N11 C24 C33 116.3(6) . .
C14 C24 C33 120.9(7) . .
O5 C25 C30 111.2(6) . .
C32 C27 C20 119.6(7) . .
C13 C28 C17 118.7(7) . 1_455
N12 C29 C32 120.9(7) . .
N12 C29 C16 117.7(6) . .
C32 C29 C16 121.4(7) . .
N12 C30 C20 122.1(7) . .
N12 C30 C25 117.1(6) . .
C20 C30 C25 120.9(7) . .
C14 C31 C18 118.1(7) . .
C27 C32 C29 119.6(7) . .
O6 C33 C24 111.6(6) . .
C23 N9 C17 118.8(6) 1_655 .
C23 N9 Co2 109.6(4) 1_655 .
C17 N9 Co2 130.0(5) . .
O8 N10 O3 123.2(7) . .
O8 N10 O4 120.3(7) . .
O3 N10 O4 116.6(6) . .
C24 N11 C15 118.0(6) . .
C24 N11 Co2 110.9(5) . .
C15 N11 Co2 130.3(5) . .
C30 N12 C29 119.5(6) . .
C30 N12 Co1 112.0(5) . .
C29 N12 Co1 128.4(5) . .
N10 O3 Co1 94.0(4) . .
N10 O4 Co1 91.4(4) . .
C25 O5 Co1 111.7(4) . .
C25 O5 Co2 121.9(4) . .
Co1 O5 Co2 92.54(19) . .
C25 O5 Co2 127.5(4) . 2_666
Co1 O5 Co2 95.41(19) . 2_666
Co2 O5 Co2 99.74(19) . 2_666
C33 O6 Co1 123.3(4) . .
C33 O6 Co2 113.3(4) . .
Co1 O6 Co2 100.8(2) . .
C22 O7 Co2 120.3(4) . 2_666
C22 O7 Co1 131.7(4) . .
Co2 O7 Co1 106.4(2) 2_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O6 1.974(5) .
Co1 O7 1.987(5) .
Co1 O5 2.097(5) .
Co1 N12 2.168(6) .
Co1 O3 2.195(5) .
Co1 O4 2.241(5) .
Co2 O7 1.975(5) 2_666
Co2 O6 2.030(5) .
Co2 O5 2.172(5) .
Co2 N11 2.180(6) .
Co2 O5 2.193(5) 2_666
Co2 N9 2.216(6) .
C13 C21 1.371(10) .
C13 C28 1.389(11) .
C14 C31 1.385(11) .
C14 C24 1.393(10) .
C15 N11 1.372(9) .
C15 C18 1.384(11) .
C15 C26 1.506(11) .
C16 C29 1.505(11) .
C17 N9 1.359(9) .
C17 C28 1.402(10) 1_655
C17 C19 1.499(10) .
C18 C31 1.389(12) .
C20 C27 1.391(11) .
C20 C30 1.394(10) .
C21 C23 1.398(10) .
C22 O7 1.402(8) .
C22 C23 1.523(9) 2_566
C23 N9 1.344(9) 1_455
C23 C22 1.523(9) 2_566
C24 N11 1.347(9) .
C24 C33 1.505(10) .
C25 O5 1.406(8) .
C25 C30 1.518(9) .
C27 C32 1.378(12) .
C28 C17 1.402(10) 1_455
C29 N12 1.354(9) .
C29 C32 1.394(10) .
C30 N12 1.345(9) .
C33 O6 1.408(8) .
N9 C23 1.344(9) 1_655
N10 O8 1.234(8) .
N10 O3 1.254(8) .
N10 O4 1.272(8) .
O5 Co2 2.193(5) 2_666
O7 Co2 1.975(5) 2_666
