#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:21:20 +0100 (vie 25 de mar de 2016) $
#$Revision: 179748 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/44/7004441.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_7004441
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 H22 Cl3 Co N4 O4 Zn'
_chemical_formula_weight         613.07
_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                95.303(4)
_cell_angle_beta                 103.086(4)
_cell_angle_gamma                107.175(5)
_cell_formula_units_Z            2
_cell_length_a                   8.2809(8)
_cell_length_b                   11.2581(10)
_cell_length_c                   13.7533(11)
_cell_measurement_reflns_used    5709
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      32.77
_cell_measurement_theta_min      2.67
_cell_volume                     1175.59(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 0.900
_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  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26030
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.34
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    2.102
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.836884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         8215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0348
_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)+(0.0291P)²+1.0224P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                6676
_reflns_number_total             8215
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b806981f.txt
_cod_data_source_block           lmzn2
_cod_original_cell_volume        1175.59(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004441
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 0.46445(3) 0.78956(2) 0.798032(16) 0.01628(5) Uani 1 1 d . . .
Co1 Co 0.18521(3) 0.33303(2) 0.782307(17) 0.01071(5) Uani 1 1 d . . .
Cl3 Cl 0.68051(7) 0.95151(5) 0.90623(4) 0.02653(11) Uani 1 1 d . . .
Cl2 Cl 0.19925(6) 0.81510(5) 0.78376(4) 0.02514(10) Uani 1 1 d . . .
Cl1 Cl 0.51592(8) 0.75300(7) 0.64673(4) 0.03927(15) Uani 1 1 d . . .
N3 N 0.35979(18) 0.28586(13) 0.73332(11) 0.0125(3) Uani 1 1 d . . .
O3 O 0.47177(17) 0.64649(12) 0.87249(10) 0.0173(2) Uani 1 1 d . . .
O1 O 0.36343(15) 0.44588(11) 0.89105(9) 0.0132(2) Uani 1 1 d . . .
O2 O 0.25648(16) 0.49985(11) 0.75032(9) 0.0147(2) Uani 1 1 d . . .
N2 N 0.01146(19) 0.21956(15) 0.66332(11) 0.0150(3) Uani 1 1 d . . .
N4 N 0.01121(19) 0.36145(14) 0.84348(12) 0.0159(3) Uani 1 1 d . . .
N1 N 0.16083(19) 0.18763(14) 0.84885(11) 0.0139(3) Uani 1 1 d . . .
C10 C 0.4063(2) 0.19563(16) 0.77889(14) 0.0143(3) Uani 1 1 d . . .
C4 C -0.0345(2) 0.09812(17) 0.67770(14) 0.0167(3) Uani 1 1 d . . .
C18 C -0.2036(2) 0.4522(2) 0.87032(17) 0.0274(5) Uani 1 1 d . . .
H18 H -0.2666 0.5068 0.8534 0.033 Uiso 1 1 calc R . .
C3 C 0.1146(3) 0.22350(19) 0.94454(14) 0.0202(4) Uani 1 1 d . . .
H3A H 0.0600 0.1484 0.9699 0.024 Uiso 1 1 calc R . .
H3B H 0.2195 0.2747 0.9962 0.024 Uiso 1 1 calc R . .
C15 C -0.0100(2) 0.29646(18) 0.92006(14) 0.0182(3) Uani 1 1 d . . .
C12 C 0.5813(2) 0.1802(2) 0.66590(16) 0.0251(4) Uani 1 1 d . . .
H12 H 0.6539 0.1427 0.6417 0.030 Uiso 1 1 calc R . .
C2 C 0.3342(2) 0.16678(18) 0.86797(14) 0.0171(3) Uani 1 1 d . . .
H2A H 0.3204 0.0800 0.8761 0.021 Uiso 1 1 calc R . .
H2B H 0.4138 0.2216 0.9294 0.021 Uiso 1 1 calc R . .
C17 C -0.2284(3) 0.3849(2) 0.94704(17) 0.0303(5) Uani 1 1 d . . .
H17 H -0.3097 0.3929 0.9819 0.036 Uiso 1 1 calc R . .
C8 C -0.0466(2) 0.2455(2) 0.56996(14) 0.0213(4) Uani 1 1 d . . .
C20 C 0.3690(2) 0.53715(16) 0.83871(13) 0.0138(3) Uani 1 1 d . . .
C14 C 0.4251(2) 0.32710(18) 0.65733(14) 0.0173(3) Uani 1 1 d . . .
H14 H 0.3939 0.3910 0.6279 0.021 Uiso 1 1 calc R . .
C19 C -0.0833(2) 0.43791(18) 0.81836(15) 0.0212(4) Uani 1 1 d . . .
H19 H -0.0679 0.4819 0.7654 0.025 Uiso 1 1 calc R . .
C11 C 0.5171(2) 0.13961(18) 0.74580(16) 0.0201(4) Uani 1 1 d . . .
H11 H 0.5475 0.0763 0.7766 0.024 Uiso 1 1 calc R . .
O4 O -0.1870(3) 0.6139(2) 0.6535(2) 0.0637(6) Uani 1 1 d . . .
C7 C -0.1486(3) 0.1455(2) 0.49005(16) 0.0294(5) Uani 1 1 d . . .
H7 H -0.1893 0.1629 0.4260 0.035 Uiso 1 1 calc R . .
C5 C -0.1335(3) -0.0019(2) 0.60061(17) 0.0266(4) Uani 1 1 d . . .
H5 H -0.1622 -0.0845 0.6128 0.032 Uiso 1 1 calc R . .
C1 C 0.0178(2) 0.07596(17) 0.78344(15) 0.0186(3) Uani 1 1 d . . .
H1A H 0.0571 0.0029 0.7834 0.022 Uiso 1 1 calc R . .
H1B H -0.0831 0.0581 0.8110 0.022 Uiso 1 1 calc R . .
C6 C -0.1885(3) 0.0241(2) 0.50521(18) 0.0322(5) Uani 1 1 d . . .
H6 H -0.2529 -0.0414 0.4513 0.039 Uiso 1 1 calc R . .
C16 C -0.1321(3) 0.3046(2) 0.97267(16) 0.0263(4) Uani 1 1 d . . .
H16 H -0.1490 0.2575 1.0238 0.032 Uiso 1 1 calc R . .
C9 C -0.0076(3) 0.3764(2) 0.55278(16) 0.0276(4) Uani 1 1 d . . .
H9A H -0.0367 0.4250 0.6033 0.041 Uiso 1 1 calc R . .
H9B H -0.0756 0.3784 0.4868 0.041 Uiso 1 1 calc R . .
H9C H 0.1149 0.4116 0.5570 0.041 Uiso 1 1 calc R . .
C13 C 0.5385(2) 0.2760(2) 0.62193(15) 0.0234(4) Uani 1 1 d . . .
H13 H 0.5846 0.3055 0.5697 0.028 Uiso 1 1 calc R . .
H101 H -0.296(8) 0.648(5) 0.648(4) 0.16(2) Uiso 1 1 d . . .
H102 H -0.060(7) 0.687(5) 0.698(4) 0.133(18) Uiso 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'
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 Cl1 110.59(4) . . ?
O3 Zn1 Cl3 101.15(4) . . ?
Cl1 Zn1 Cl3 113.13(2) . . ?
O3 Zn1 Cl2 107.93(4) . . ?
Cl1 Zn1 Cl2 112.17(2) . . ?
Cl3 Zn1 Cl2 111.23(2) . . ?
O1 Co1 N3 89.55(6) . . ?
O1 Co1 N4 89.95(6) . . ?
N3 Co1 N4 171.54(6) . . ?
O1 Co1 O2 69.03(5) . . ?
N3 Co1 O2 93.56(6) . . ?
N4 Co1 O2 94.15(6) . . ?
O1 Co1 N1 95.33(6) . . ?
N3 Co1 N1 86.26(6) . . ?
N4 Co1 N1 85.38(6) . . ?
O2 Co1 N1 164.35(6) . . ?
O1 Co1 N2 175.93(6) . . ?
N3 Co1 N2 87.29(6) . . ?
N4 Co1 N2 93.55(6) . . ?
O2 Co1 N2 108.61(6) . . ?
N1 Co1 N2 87.03(6) . . ?
O1 Co1 C20 34.61(6) . . ?
N3 Co1 C20 91.64(6) . . ?
N4 Co1 C20 92.73(6) . . ?
O2 Co1 C20 34.42(6) . . ?
N1 Co1 C20 129.94(6) . . ?
N2 Co1 C20 142.90(6) . . ?
C14 N3 C10 120.62(15) . . ?
C14 N3 Co1 126.60(12) . . ?
C10 N3 Co1 112.61(11) . . ?
C20 O3 Zn1 122.17(12) . . ?
C20 O1 Co1 89.98(10) . . ?
C20 O2 Co1 88.86(10) . . ?
C4 N2 C8 118.98(16) . . ?
C4 N2 Co1 111.84(12) . . ?
C8 N2 Co1 128.62(14) . . ?
C19 N4 C15 120.30(16) . . ?
C19 N4 Co1 126.62(13) . . ?
C15 N4 Co1 113.07(12) . . ?
C1 N1 C2 111.58(14) . . ?
C1 N1 C3 110.27(14) . . ?
C2 N1 C3 113.16(14) . . ?
C1 N1 Co1 110.36(11) . . ?
C2 N1 Co1 105.91(10) . . ?
C3 N1 Co1 105.26(11) . . ?
N3 C10 C11 120.90(17) . . ?
N3 C10 C2 114.47(15) . . ?
C11 C10 C2 124.59(16) . . ?
N2 C4 C5 122.99(18) . . ?
N2 C4 C1 116.74(16) . . ?
C5 C4 C1 120.17(18) . . ?
C17 C18 C19 119.2(2) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C15 C3 N1 107.83(15) . . ?
C15 C3 H3A 110.1 . . ?
N1 C3 H3A 110.1 . . ?
C15 C3 H3B 110.1 . . ?
N1 C3 H3B 110.1 . . ?
H3A C3 H3B 108.5 . . ?
N4 C15 C16 121.08(19) . . ?
N4 C15 C3 114.06(15) . . ?
C16 C15 C3 124.78(18) . . ?
C13 C12 C11 120.48(17) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
N1 C2 C10 107.97(14) . . ?
N1 C2 H2A 110.1 . . ?
C10 C2 H2A 110.1 . . ?
N1 C2 H2B 110.1 . . ?
C10 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
C18 C17 C16 120.04(18) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
N2 C8 C7 119.27(19) . . ?
N2 C8 C9 120.53(18) . . ?
C7 C8 C9 120.18(19) . . ?
O3 C20 O2 125.64(16) . . ?
O3 C20 O1 122.23(16) . . ?
O2 C20 O1 112.13(15) . . ?
O3 C20 Co1 177.62(14) . . ?
O2 C20 Co1 56.73(8) . . ?
O1 C20 Co1 55.41(8) . . ?
N3 C14 C13 121.06(17) . . ?
N3 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
N4 C19 C18 121.0(2) . . ?
N4 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C12 C11 C10 118.39(18) . . ?
C12 C11 H11 120.8 . . ?
C10 C11 H11 120.8 . . ?
H101 O4 H102 112(4) . . ?
C6 C7 C8 120.9(2) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C6 C5 C4 118.1(2) . . ?
C6 C5 H5 121.0 . . ?
C4 C5 H5 121.0 . . ?
C4 C1 N1 111.37(15) . . ?
C4 C1 H1A 109.4 . . ?
N1 C1 H1A 109.4 . . ?
C4 C1 H1B 109.4 . . ?
N1 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C7 C6 C5 119.8(2) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C15 C16 C17 118.4(2) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C13 C14 118.48(18) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
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 1.9954(13) . ?
Zn1 Cl1 2.2423(6) . ?
Zn1 Cl3 2.2597(6) . ?
Zn1 Cl2 2.2654(6) . ?
Co1 O1 1.8896(12) . ?
Co1 N3 1.9116(14) . ?
Co1 N4 1.9126(14) . ?
Co1 O2 1.9195(12) . ?
Co1 N1 1.9296(15) . ?
Co1 N2 1.9601(15) . ?
Co1 C20 2.2954(18) . ?
N3 C14 1.341(2) . ?
N3 C10 1.346(2) . ?
O3 C20 1.246(2) . ?
O1 C20 1.304(2) . ?
O2 C20 1.298(2) . ?
N2 C4 1.353(2) . ?
N2 C8 1.356(2) . ?
N4 C19 1.343(2) . ?
N4 C15 1.351(2) . ?
N1 C1 1.491(2) . ?
N1 C2 1.491(2) . ?
N1 C3 1.504(2) . ?
C10 C11 1.387(2) . ?
C10 C2 1.501(2) . ?
C4 C5 1.380(3) . ?
C4 C1 1.487(3) . ?
C18 C17 1.373(3) . ?
C18 C19 1.387(3) . ?
C18 H18 0.9300 . ?
C3 C15 1.499(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C15 C16 1.389(2) . ?
C12 C13 1.379(3) . ?
C12 C11 1.383(3) . ?
C12 H12 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C17 C16 1.391(3) . ?
C17 H17 0.9300 . ?
C8 C7 1.406(3) . ?
C8 C9 1.466(3) . ?
C14 C13 1.387(3) . ?
C14 H14 0.9300 . ?
C19 H19 0.9300 . ?
C11 H11 0.9300 . ?
O4 H101 1.07(6) . ?
O4 H102 1.13(6) . ?
C7 C6 1.357(3) . ?
C7 H7 0.9300 . ?
C5 C6 1.376(3) . ?
C5 H5 0.9300 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C6 H6 0.9300 . ?
C16 H16 0.9300 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C13 H13 0.9300 . ?
