#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/08/2210887.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2210887
loop_
_publ_author_name
'Duriska, Martin B.'
'Batten, Stuart R.'
_publ_section_title
;
 (1,4,10,13-Tetraoxa-7,16-diazacyclooctadecane-7,16-diacetato)cobalt(II)
;
_journal_coeditor_code           BI2082
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2928
_journal_page_last               m2929
_journal_paper_doi               10.1107/S1600536806042097
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Co (C16 H28 N2 O8)]'
_chemical_formula_moiety         'C16 H28 Co N2 O8'
_chemical_formula_sum            'C16 H28 Co N2 O8'
_chemical_formula_weight         435.33
_chemical_name_systematic
;
(1,4,10,13-Tetraoxa-7,16-diazacyclooctadecane-7,16-diacetato)cobalt(II)
;
_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                79.851(2)
_cell_angle_beta                 69.746(2)
_cell_angle_gamma                86.440(2)
_cell_formula_units_Z            1
_cell_length_a                   6.8973(5)
_cell_length_b                   7.5264(5)
_cell_length_c                   9.1052(7)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.427
_cell_measurement_theta_min      2.418
_cell_volume                     436.50(5)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'X-SEED (Barbour, 1999)'
_computing_publication_material  X-SEED
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker X8 APEX-II CCD'
_diffrn_measurement_method       'φ and ω'
_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  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4881
_diffrn_reflns_theta_full        28.44
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         2.42
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            'pale purple'
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             229
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0250
_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)+(0.0182P)²+0.3282P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                2099
_reflns_number_total             2177
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bi2082.cif
_cod_data_source_block           I
_cod_database_code               2210887
_cod_database_fobs_code          2210887
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Co Co1 0.5000 0.0000 0.0000 0.01016(7) Uani d S 1
O O1 0.45386(15) -0.23261(12) 0.42526(11) 0.01266(19) Uani d . 1
N N1 0.55978(17) 0.11021(14) 0.18156(13) 0.0099(2) Uani d . 1
C C1 0.3334(2) -0.37202(17) 0.41396(16) 0.0132(3) Uani d . 1
H H1B 0.2460 -0.4262 0.5223 0.016 Uiso calc R 1
H H1A 0.4272 -0.4674 0.3663 0.016 Uiso calc R 1
O O2 0.68587(15) 0.26844(13) -0.15063(11) 0.01311(19) Uani d . 1
C C2 0.6458(2) -0.19912(17) 0.29804(15) 0.0124(2) Uani d . 1
H H2A 0.6380 -0.2413 0.2032 0.015 Uiso calc R 1
H H2B 0.7575 -0.2669 0.3285 0.015 Uiso calc R 1
O O3 0.23440(15) 0.13282(13) 0.07986(11) 0.01356(19) Uani d . 1
C C3 0.6940(2) -0.00040(17) 0.25936(15) 0.0116(2) Uani d . 1
H H3B 0.6799 0.0439 0.3587 0.014 Uiso calc R 1
H H3A 0.8397 0.0170 0.1887 0.014 Uiso calc R 1
O O4 0.04622(15) 0.28279(14) 0.27196(12) 0.0175(2) Uani d . 1
C C4 0.6585(2) 0.29051(17) 0.11065(15) 0.0122(2) Uani d . 1
H H4A 0.7329 0.3228 0.1777 0.015 Uiso calc R 1
H H4B 0.5498 0.3825 0.1091 0.015 Uiso calc R 1
C C5 0.8067(2) 0.29279(18) -0.05469(16) 0.0131(3) Uani d . 1
H H5B 0.8814 0.4092 -0.0948 0.016 Uiso calc R 1
H H5A 0.9091 0.1942 -0.0570 0.016 Uiso calc R 1
C C7 0.3527(2) 0.14072(17) 0.29532(15) 0.0115(2) Uani d . 1
H H7B 0.3606 0.2378 0.3536 0.014 Uiso calc R 1
H H7A 0.3054 0.0293 0.3736 0.014 Uiso calc R 1
C C8 0.1975(2) 0.19353(17) 0.20988(15) 0.0116(2) Uani d . 1
C C9 0.8035(2) 0.31109(18) -0.31712(15) 0.0139(3) Uani d . 1
H H9A 0.8824 0.2032 -0.3533 0.017 Uiso calc R 1
H H9B 0.9038 0.4078 -0.3341 0.017 Uiso calc R 1
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Co1 O2 . . 78.98(4) y
N1 Co1 O2 . 2_655 101.02(4) y
N1 Co1 O3 . . 81.13(4) y
O2 Co1 O3 . . 93.19(4) y
O3 Co1 N1 . 2_655 98.87(4) y
O3 Co1 O2 . 2_655 86.81(4) y
O3 Co1 O3 2_655 . 180.00(6) ?
O3 Co1 N1 2_655 2_655 81.13(4) ?
O3 Co1 N1 2_655 . 98.87(4) ?
N1 Co1 N1 2_655 . 180.00(8) ?
O3 Co1 O2 2_655 2_655 93.19(4) ?
N1 Co1 O2 2_655 2_655 78.98(4) ?
O3 Co1 O2 2_655 . 86.81(4) ?
N1 Co1 O2 2_655 . 101.02(4) ?
O2 Co1 O2 2_655 . 180.00(6) ?
C1 O1 C2 . . 114.84(10) ?
C7 N1 C3 . . 112.37(10) ?
C7 N1 C4 . . 107.30(10) ?
C3 N1 C4 . . 108.16(10) ?
C7 N1 Co1 . . 104.54(7) ?
C3 N1 Co1 . . 115.74(8) ?
C4 N1 Co1 . . 108.38(8) ?
O1 C1 C9 . 2_655 114.23(11) ?
O1 C1 H1B . . 108.7 ?
C9 C1 H1B 2_655 . 108.7 ?
O1 C1 H1A . . 108.7 ?
C9 C1 H1A 2_655 . 108.7 ?
H1B C1 H1A . . 107.6 ?
C9 O2 C5 . . 111.39(10) ?
C9 O2 Co1 . . 130.14(8) ?
C5 O2 Co1 . . 100.34(7) ?
O1 C2 C3 . . 110.10(10) ?
O1 C2 H2A . . 109.6 ?
C3 C2 H2A . . 109.6 ?
O1 C2 H2B . . 109.6 ?
C3 C2 H2B . . 109.6 ?
H2A C2 H2B . . 108.2 ?
C8 O3 Co1 . . 117.15(8) ?
N1 C3 C2 . . 114.05(10) ?
N1 C3 H3B . . 108.7 ?
C2 C3 H3B . . 108.7 ?
N1 C3 H3A . . 108.7 ?
C2 C3 H3A . . 108.7 ?
H3B C3 H3A . . 107.6 ?
N1 C4 C5 . . 111.91(10) ?
N1 C4 H4A . . 109.2 ?
C5 C4 H4A . . 109.2 ?
N1 C4 H4B . . 109.2 ?
C5 C4 H4B . . 109.2 ?
H4A C4 H4B . . 107.9 ?
O2 C5 C4 . . 106.70(11) ?
O2 C5 H5B . . 110.4 ?
C4 C5 H5B . . 110.4 ?
O2 C5 H5A . . 110.4 ?
C4 C5 H5A . . 110.4 ?
H5B C5 H5A . . 108.6 ?
N1 C7 C8 . . 110.96(10) ?
N1 C7 H7B . . 109.4 ?
C8 C7 H7B . . 109.4 ?
N1 C7 H7A . . 109.4 ?
C8 C7 H7A . . 109.4 ?
H7B C7 H7A . . 108.0 ?
O4 C8 O3 . . 125.43(13) ?
O4 C8 C7 . . 118.59(12) ?
O3 C8 C7 . . 115.91(11) ?
O2 C9 C1 . 2_655 111.64(11) ?
O2 C9 H9A . . 109.3 ?
C1 C9 H9A 2_655 . 109.3 ?
O2 C9 H9B . . 109.3 ?
C1 C9 H9B 2_655 . 109.3 ?
H9A C9 H9B . . 108.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 N1 . 2.1421(11) y
Co1 O2 . 2.3946(9) y
Co1 O3 . 1.9976(10) y
Co1 N1 2_655 2.1421(11) ?
Co1 O2 2_655 2.3946(9) ?
Co1 O3 2_655 1.9976(10) ?
O1 C1 . 1.4168(15) ?
O1 C2 . 1.4264(16) ?
N1 C7 . 1.4781(16) ?
N1 C3 . 1.4842(16) ?
N1 C4 . 1.4911(16) ?
C1 C9 2_655 1.5032(19) ?
C1 H1B . 0.990 ?
C1 H1A . 0.990 ?
O2 C9 . 1.4383(15) ?
O2 C5 . 1.4389(15) ?
C2 C3 . 1.5056(17) ?
C2 H2A . 0.990 ?
C2 H2B . 0.990 ?
O3 C8 . 1.2816(16) ?
C3 H3B . 0.990 ?
C3 H3A . 0.990 ?
O4 C8 . 1.2241(16) ?
C4 C5 . 1.4965(18) ?
C4 H4A . 0.990 ?
C4 H4B . 0.990 ?
C5 H5B . 0.990 ?
C5 H5A . 0.990 ?
C7 C8 . 1.5241(18) ?
C7 H7B . 0.990 ?
C7 H7A . 0.990 ?
C9 C1 2_655 1.5032(19) ?
C9 H9A . 0.990 ?
C9 H9B . 0.990 ?
