#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:21:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179748 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/44/7004442.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_7004442
loop_
_publ_author_name
'McClintock, Lisa F.'
'Cavigliasso, Germán'
'Stranger, Robert'
'Blackman, Allan G.'
_publ_section_title
;
 The donor ability of the chelated carbonate ligand: protonation and
 metallation of [(L)Co(O2CO)]+ complexes in aqueous solution
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              4984
_journal_page_last               4992
_journal_paper_doi               10.1039/b806981f
_journal_year                    2008
_chemical_formula_sum            'C20 H20 Cl3 Co N4 O3 Zn'
_chemical_formula_weight         595.05
_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                95.851(4)
_cell_angle_beta                 102.607(4)
_cell_angle_gamma                108.600(4)
_cell_formula_units_Z            2
_cell_length_a                   8.2916(7)
_cell_length_b                   11.0966(11)
_cell_length_c                   14.0994(13)
_cell_measurement_reflns_used    7611
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      34.38
_cell_measurement_theta_min      2.69
_cell_volume                     1179.04(19)
_computing_cell_refinement       'ApexII and SAINT (Bruker, 2001)'
_computing_data_collection       'ApexII (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'WinGX (Farrugia, 1999)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Bruker Kappa ApexII area detector'
_diffrn_measurement_method       'phi and omega 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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20348
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         34.74
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    2.090
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.769623
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   SQUEEZE
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         9494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0347
_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)+(0.0378P)²+0.0235P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                7372
_reflns_number_total             9494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b806981f.txt
_cod_data_source_block           lma3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004442
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.02176(2) -0.295998(18) 0.190646(13) 0.01414(5) Uani 1 1 d . . .
Co1 Co 0.32102(2) 0.173196(19) 0.218723(14) 0.00934(5) Uani 1 1 d . . .
Cl1 Cl -0.06493(6) -0.28812(5) 0.33233(3) 0.02773(10) Uani 1 1 d . . .
Cl2 Cl 0.29889(5) -0.30144(4) 0.21682(3) 0.02084(8) Uani 1 1 d . . .
Cl3 Cl -0.17735(5) -0.46367(4) 0.07616(3) 0.02084(8) Uani 1 1 d . . .
O1 O 0.13625(13) 0.05935(10) 0.11051(8) 0.0120(2) Uani 1 1 d . . .
O2 O 0.23656(14) 0.00243(10) 0.24721(8) 0.0130(2) Uani 1 1 d . . .
O3 O 0.01421(14) -0.14596(11) 0.12606(8) 0.0167(2) Uani 1 1 d . . .
N2 N 0.15190(16) 0.22479(13) 0.26783(9) 0.0118(2) Uani 1 1 d . . .
N3 N 0.49233(16) 0.13943(13) 0.15777(9) 0.0121(2) Uani 1 1 d . . .
C10 C 0.10244(19) 0.31243(15) 0.22073(11) 0.0133(3) Uani 1 1 d . . .
N1 N 0.35287(17) 0.32082(13) 0.15276(10) 0.0143(2) Uani 1 1 d . . .
C6 C 0.6612(2) 0.43923(17) 0.47536(12) 0.0194(3) Uani 1 1 d . . .
H6 H 0.7045 0.5282 0.4981 0.023 Uiso 1 1 calc R . .
C8 C 0.6400(2) 0.22709(19) 0.50162(12) 0.0215(3) Uani 1 1 d . . .
H8 H 0.6672 0.1709 0.5417 0.026 Uiso 1 1 calc R . .
N4 N 0.49133(16) 0.25891(13) 0.34543(9) 0.0128(2) Uani 1 1 d . . .
C3 C 0.17927(19) 0.34271(16) 0.13492(12) 0.0156(3) Uani 1 1 d . . .
H3A H 0.1973 0.4320 0.1285 0.019 Uiso 1 1 calc R . .
H3B H 0.0986 0.2873 0.0741 0.019 Uiso 1 1 calc R . .
C4 C 0.3929(2) 0.27744(17) 0.05784(11) 0.0173(3) Uani 1 1 d . . .
H4A H 0.2846 0.2232 0.0092 0.021 Uiso 1 1 calc R . .
H4B H 0.4488 0.3520 0.0308 0.021 Uiso 1 1 calc R . .
C16 C 0.6353(2) 0.19142(18) 0.03019(12) 0.0203(3) Uani 1 1 d . . .
H16 H 0.6523 0.2368 -0.0209 0.024 Uiso 1 1 calc R . .
C5 C 0.55213(18) 0.38779(15) 0.37942(11) 0.0141(3) Uani 1 1 d . . .
C15 C 0.5152(2) 0.20240(15) 0.08196(11) 0.0147(3) Uani 1 1 d . . .
C18 C 0.7043(2) 0.04542(17) 0.13287(13) 0.0212(3) Uani 1 1 d . . .
H18 H 0.7667 -0.0088 0.1505 0.025 Uiso 1 1 calc R . .
C11 C -0.0086(2) 0.36892(17) 0.25224(13) 0.0193(3) Uani 1 1 d . . .
H11 H -0.0440 0.4282 0.2190 0.023 Uiso 1 1 calc R . .
C19 C 0.5841(2) 0.06171(16) 0.18305(12) 0.0165(3) Uani 1 1 d . . .
H19 H 0.5665 0.0182 0.2350 0.020 Uiso 1 1 calc R . .
C12 C -0.0653(2) 0.33467(19) 0.33454(13) 0.0227(4) Uani 1 1 d . . .
H12 H -0.1375 0.3726 0.3581 0.027 Uiso 1 1 calc R . .
C20 C 0.12395(19) -0.03383(15) 0.16001(11) 0.0121(3) Uani 1 1 d . . .
C2 C 0.5029(2) 0.47586(16) 0.31401(12) 0.0164(3) Uani 1 1 d . . .
H2A H 0.5854 0.5634 0.3403 0.020 Uiso 1 1 calc R . .
H2B H 0.3864 0.4752 0.3160 0.020 Uiso 1 1 calc R . .
C17 C 0.7298(2) 0.11120(18) 0.05622(13) 0.0233(4) Uani 1 1 d . . .
H17 H 0.8103 0.1017 0.0220 0.028 Uiso 1 1 calc R . .
C9 C 0.5343(2) 0.18020(17) 0.40617(12) 0.0171(3) Uani 1 1 d . . .
H9 H 0.4909 0.0914 0.3826 0.021 Uiso 1 1 calc R . .
C14 C 0.0938(2) 0.18929(17) 0.34595(11) 0.0165(3) Uani 1 1 d . . .
H14 H 0.1266 0.1271 0.3765 0.020 Uiso 1 1 calc R . .
C7 C 0.7047(2) 0.35844(19) 0.53648(12) 0.0223(4) Uani 1 1 d . . .
H7 H 0.7769 0.3924 0.6004 0.027 Uiso 1 1 calc R . .
C1 C 0.5020(2) 0.44015(16) 0.20775(11) 0.0158(3) Uani 1 1 d . . .
H1A H 0.4960 0.5114 0.1743 0.019 Uiso 1 1 calc R . .
H1B H 0.6122 0.4279 0.2062 0.019 Uiso 1 1 calc R . .
C13 C -0.0143(2) 0.24410(19) 0.38141(13) 0.0221(4) Uani 1 1 d . . .
H13 H -0.0525 0.2203 0.4363 0.027 Uiso 1 1 calc 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'
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'
Zn Zn 0.2839 1.4301 '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
O3 Zn1 Cl3 102.05(3) . . ?
O3 Zn1 Cl2 108.20(4) . . ?
Cl3 Zn1 Cl2 112.388(18) . . ?
O3 Zn1 Cl1 112.02(4) . . ?
Cl3 Zn1 Cl1 109.716(19) . . ?
Cl2 Zn1 Cl1 112.066(17) . . ?
O1 Co1 N2 89.59(5) . . ?
O1 Co1 O2 69.06(5) . . ?
N2 Co1 O2 93.22(5) . . ?
O1 Co1 N3 89.78(5) . . ?
N2 Co1 N3 171.92(6) . . ?
O2 Co1 N3 94.07(5) . . ?
O1 Co1 N1 93.67(5) . . ?
N2 Co1 N1 86.55(6) . . ?
O2 Co1 N1 162.73(5) . . ?
N3 Co1 N1 85.45(6) . . ?
O1 Co1 N4 167.19(5) . . ?
N2 Co1 N4 87.98(5) . . ?
O2 Co1 N4 98.52(5) . . ?
N3 Co1 N4 94.37(5) . . ?
N1 Co1 N4 98.73(6) . . ?
O1 Co1 C20 34.38(5) . . ?
N2 Co1 C20 91.60(5) . . ?
O2 Co1 C20 34.68(5) . . ?
N3 Co1 C20 92.42(5) . . ?
N1 Co1 C20 128.05(5) . . ?
N4 Co1 C20 133.12(6) . . ?
C20 O1 Co1 89.53(8) . . ?
C20 O2 Co1 88.65(9) . . ?
C20 O3 Zn1 122.57(10) . . ?
C14 N2 C10 120.75(13) . . ?
C14 N2 Co1 125.90(11) . . ?
C10 N2 Co1 113.14(10) . . ?
C19 N3 C15 120.18(14) . . ?
C19 N3 Co1 126.73(11) . . ?
C15 N3 Co1 113.09(10) . . ?
N2 C10 C11 120.96(15) . . ?
N2 C10 C3 114.49(13) . . ?
C11 C10 C3 124.55(15) . . ?
C1 N1 C3 111.33(12) . . ?
C1 N1 C4 107.85(12) . . ?
C3 N1 C4 112.83(12) . . ?
C1 N1 Co1 115.02(10) . . ?
C3 N1 Co1 105.29(9) . . ?
C4 N1 Co1 104.44(10) . . ?
C7 C6 C5 120.20(16) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C7 C8 C9 118.85(16) . . ?
C7 C8 H8 120.6 . . ?
C9 C8 H8 120.6 . . ?
C5 N4 C9 119.23(13) . . ?
C5 N4 Co1 124.27(11) . . ?
C9 N4 Co1 116.09(11) . . ?
C10 C3 N1 108.84(12) . . ?
C10 C3 H3A 109.9 . . ?
N1 C3 H3A 109.9 . . ?
C10 C3 H3B 109.9 . . ?
N1 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
C15 C4 N1 107.81(12) . . ?
C15 C4 H4A 110.1 . . ?
N1 C4 H4A 110.1 . . ?
C15 C4 H4B 110.1 . . ?
N1 C4 H4B 110.1 . . ?
H4A C4 H4B 108.5 . . ?
C15 C16 C17 118.52(17) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
N4 C5 C6 120.14(15) . . ?
N4 C5 C2 119.93(13) . . ?
C6 C5 C2 119.92(15) . . ?
N3 C15 C16 121.27(15) . . ?
N3 C15 C4 113.76(13) . . ?
C16 C15 C4 124.90(15) . . ?
C17 C18 C19 118.83(16) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C12 C11 C10 118.35(16) . . ?
C12 C11 H11 120.8 . . ?
C10 C11 H11 120.8 . . ?
N3 C19 C18 121.10(16) . . ?
N3 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C13 C12 C11 119.87(15) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
O3 C20 O1 122.43(13) . . ?
O3 C20 O2 124.81(14) . . ?
O1 C20 O2 112.76(13) . . ?
O3 C20 Co1 178.50(12) . . ?
O1 C20 Co1 56.09(7) . . ?
O2 C20 Co1 56.67(7) . . ?
C5 C2 C1 114.16(13) . . ?
C5 C2 H2A 108.7 . . ?
C1 C2 H2A 108.7 . . ?
C5 C2 H2B 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C18 C17 C16 120.08(16) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
N4 C9 C8 122.36(16) . . ?
N4 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
N2 C14 C13 120.66(16) . . ?
N2 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C8 C7 C6 119.21(15) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
N1 C1 C2 113.57(13) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C14 C13 C12 119.38(16) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
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
Zn1 O3 1.9889(12) . ?
Zn1 Cl3 2.2490(5) . ?
Zn1 Cl2 2.2678(5) . ?
Zn1 Cl1 2.2686(5) . ?
Co1 O1 1.9034(10) . ?
Co1 N2 1.9049(13) . ?
Co1 O2 1.9167(11) . ?
Co1 N3 1.9244(13) . ?
Co1 N1 1.9391(14) . ?
Co1 N4 1.9458(12) . ?
Co1 C20 2.2934(15) . ?
O1 C20 1.2951(19) . ?
O2 C20 1.3052(17) . ?
O3 C20 1.2536(18) . ?
N2 C14 1.342(2) . ?
N2 C10 1.350(2) . ?
N3 C19 1.346(2) . ?
N3 C15 1.350(2) . ?
C10 C11 1.388(2) . ?
C10 C3 1.505(2) . ?
N1 C1 1.487(2) . ?
N1 C3 1.5072(19) . ?
N1 C4 1.516(2) . ?
C6 C7 1.380(3) . ?
C6 C5 1.397(2) . ?
C6 H6 0.9300 . ?
C8 C7 1.376(3) . ?
C8 C9 1.379(2) . ?
C8 H8 0.9300 . ?
N4 C5 1.351(2) . ?
N4 C9 1.357(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C15 1.511(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C16 C15 1.385(2) . ?
C16 C17 1.388(3) . ?
C16 H16 0.9300 . ?
C5 C2 1.499(2) . ?
C18 C17 1.381(3) . ?
C18 C19 1.387(2) . ?
C18 H18 0.9300 . ?
C11 C12 1.388(3) . ?
C11 H11 0.9300 . ?
C19 H19 0.9300 . ?
C12 C13 1.382(3) . ?
C12 H12 0.9300 . ?
C2 C1 1.508(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C17 H17 0.9300 . ?
C9 H9 0.9300 . ?
C14 C13 1.380(2) . ?
C14 H14 0.9300 . ?
C7 H7 0.9300 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C13 H13 0.9300 . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.500 99.4 24.3
