#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:39:42 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179801 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/97/7009722.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_7009722
loop_
_publ_author_name
'Hartshorn, Richard M.'
'Telfer, Shane G.'
_publ_section_title
;
 The photodecarboxylation of [N,N-bis(2-pyridylmethyl)amino
 acidato]phenanthrolinecobalt(III) complexes: -- formation and
 decomposition of metallacyclic species †
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2801
_journal_paper_doi               10.1039/b003095n
_journal_year                    2000
_chemical_formula_sum            'C48 H42 Cl4 Co2 N10 O18'
_chemical_formula_weight         1306.58
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.142(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.652(10)
_cell_length_b                   11.320(5)
_cell_length_c                   12.352(6)
_cell_measurement_temperature    168(2)
_cell_volume                     2763(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD 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  0.0743
_diffrn_reflns_av_sigmaI/netI    0.1397
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6574
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       thin_block
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          .04
_exptl_crystal_size_mid          .05
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.823
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.823
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0497
_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)+(0.0525P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                1194
_reflns_number_total             2287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b003095n.txt
_cod_data_source_block           stdrf
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7009722
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_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
Co Co 0.09184(5) 0.0000 0.17519(9) 0.0232(3) Uani 1 2 d S . .
O1 O 0.0021(2) 0.0000 0.0595(4) 0.0296(12) Uani 1 2 d S . .
N1 N 0.0704(2) 0.1190(4) 0.2657(4) 0.0282(11) Uani 1 1 d . . .
N2 N 0.1830(3) 0.0000 0.3119(5) 0.0270(15) Uani 1 2 d S . .
HN2 H 0.2156 0.0000 0.2810 0.032 Uiso 1 2 calc SR . .
N3 N 0.12125(19) 0.1151(4) 0.0895(3) 0.0263(11) Uani 1 1 d . . .
C1 C 0.0079(3) 0.1646(5) 0.2389(5) 0.0449(16) Uani 1 1 d . . .
H1 H -0.0291 0.1372 0.1701 0.054 Uiso 1 1 calc R . .
C2 C -0.0035(3) 0.2493(6) 0.3084(6) 0.061(2) Uani 1 1 d . . .
H2 H -0.0477 0.2795 0.2886 0.073 Uiso 1 1 calc R . .
C3 C 0.0505(3) 0.2895(5) 0.4075(6) 0.0566(19) Uani 1 1 d . . .
H3 H 0.0439 0.3499 0.4552 0.068 Uiso 1 1 calc R . .
C4 C 0.1131(3) 0.2430(5) 0.4370(5) 0.0397(15) Uani 1 1 d . . .
H4 H 0.1501 0.2682 0.5067 0.048 Uiso 1 1 calc R . .
C5 C 0.1222(3) 0.1580(4) 0.3638(5) 0.0290(13) Uani 1 1 d . . .
C6 C 0.1905(2) 0.1111(4) 0.3799(5) 0.0347(14) Uani 1 1 d . . .
H6'' H 0.2143 0.1707 0.3524 0.042 Uiso 1 1 calc R . .
H6' H 0.2181 0.0960 0.4652 0.042 Uiso 1 1 calc R . .
C7 C 0.1174(2) 0.2325(4) 0.0868(5) 0.0324(14) Uani 1 1 d . . .
H7 H 0.0993 0.2711 0.1355 0.039 Uiso 1 1 calc R . .
C8 C 0.1390(3) 0.3008(5) 0.0156(5) 0.0413(16) Uani 1 1 d . . .
H8 H 0.1352 0.3844 0.0163 0.050 Uiso 1 1 calc R . .
C9 C 0.1656(3) 0.2487(5) -0.0557(5) 0.0388(15) Uani 1 1 d . . .
H9 H 0.1807 0.2956 -0.1039 0.047 Uiso 1 1 calc R . .
C10 C 0.1703(2) 0.1259(5) -0.0565(5) 0.0310(14) Uani 1 1 d . . .
C11 C 0.1476(2) 0.0625(4) 0.0171(4) 0.0237(12) Uani 1 1 d . . .
C12 C 0.1943(2) 0.0590(5) -0.1315(5) 0.0418(16) Uani 1 1 d . . .
H12 H 0.2104 0.0999 -0.1819 0.050 Uiso 1 1 calc R . .
Cl1 Cl 0.15331(11) 0.5000 -0.27878(18) 0.0354(5) Uani 1 2 d S . .
O4 O 0.1445(3) 0.5000 -0.1703(5) 0.0654(19) Uani 1 2 d S . .
O3 O 0.1906(2) 0.6030(3) -0.2837(3) 0.0547(12) Uani 1 1 d . . .
O2 O 0.0889(3) 0.5000 -0.3754(6) 0.071(2) Uani 1 2 d S . .
Cl2 Cl 0.17955(10) 0.5000 -0.69253(18) 0.0402(6) Uani 1 2 d S . .
O8 O 0.1655(3) 0.5000 -0.5885(5) 0.0515(16) Uani 1 2 d S . .
O7 O 0.2182(2) 0.3955(3) -0.6915(3) 0.0565(12) Uani 1 1 d . . .
O6 O 0.1176(3) 0.5000 -0.7970(5) 0.071(2) Uani 1 2 d S . .
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'
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
O1 Co N1 91.23(16) . 6 ?
O1 Co N1 91.23(16) . . ?
N1 Co N1 88.9(2) 6 . ?
O1 Co N3 93.04(15) . 6 ?
N1 Co N3 93.31(17) 6 6 ?
N1 Co N3 175.17(18) . 6 ?
O1 Co N3 93.04(15) . . ?
N1 Co N3 175.17(18) 6 . ?
N1 Co N3 93.31(17) . . ?
N3 Co N3 84.2(3) 6 . ?
O1 Co N2 173.6(2) . . ?
N1 Co N2 84.20(18) 6 . ?
N1 Co N2 84.20(18) . . ?
N3 Co N2 91.72(17) 6 . ?
N3 Co N2 91.72(17) . . ?
O1 O1 Co 113.0(4) 5 . ?
C5 N1 C1 118.4(5) . . ?
C5 N1 Co 116.3(3) . . ?
C1 N1 Co 125.3(4) . . ?
C6 N2 C6 115.8(6) . 6 ?
C6 N2 Co 108.6(3) . . ?
C6 N2 Co 108.6(3) 6 . ?
C7 N3 C11 117.0(4) . . ?
C7 N3 Co 130.7(4) . . ?
C11 N3 Co 112.3(3) . . ?
N1 C1 C2 121.9(5) . . ?
C1 C2 C3 118.7(6) . . ?
C4 C3 C2 120.0(6) . . ?
C3 C4 C5 119.2(5) . . ?
N1 C5 C4 121.7(5) . . ?
N1 C5 C6 114.5(4) . . ?
C4 C5 C6 123.5(5) . . ?
N2 C6 C5 110.5(4) . . ?
N3 C7 C8 122.6(5) . . ?
C9 C8 C7 120.5(5) . . ?
C8 C9 C10 119.1(5) . . ?
C9 C10 C11 117.5(5) . . ?
C9 C10 C12 125.0(5) . . ?
C11 C10 C12 117.5(5) . . ?
N3 C11 C10 123.3(4) . . ?
N3 C11 C11 115.6(3) . 6 ?
C10 C11 C11 121.0(3) . 6 ?
C12 C12 C10 121.6(3) 6 . ?
O2 Cl1 O4 109.1(4) . . ?
O2 Cl1 O3 109.9(2) . . ?
O4 Cl1 O3 109.5(2) . . ?
O2 Cl1 O3 109.9(2) . 6_565 ?
O4 Cl1 O3 109.5(2) . 6_565 ?
O3 Cl1 O3 108.9(3) . 6_565 ?
O6 Cl2 O8 110.1(4) . . ?
O6 Cl2 O7 109.4(2) . 6_565 ?
O8 Cl2 O7 109.0(2) . 6_565 ?
O6 Cl2 O7 109.4(2) . . ?
O8 Cl2 O7 109.0(2) . . ?
O7 Cl2 O7 109.8(3) 6_565 . ?
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 O1 1.883(5) . ?
Co N1 1.925(4) 6 ?
Co N1 1.925(4) . ?
Co N3 1.943(4) 6 ?
Co N3 1.943(4) . ?
Co N2 2.004(6) . ?
O1 O1 1.436(8) 5 ?
N1 C5 1.345(6) . ?
N1 C1 1.357(6) . ?
N2 C6 1.484(5) . ?
N2 C6 1.484(5) 6 ?
N3 C7 1.332(6) . ?
N3 C11 1.377(6) . ?
C1 C2 1.375(7) . ?
C2 C3 1.380(8) . ?
C3 C4 1.357(7) . ?
C4 C5 1.388(7) . ?
C5 C6 1.506(7) . ?
C7 C8 1.387(7) . ?
C8 C9 1.367(7) . ?
C9 C10 1.394(7) . ?
C10 C11 1.397(7) . ?
C10 C12 1.448(7) . ?
C11 C11 1.414(9) 6 ?
C12 C12 1.335(11) 6 ?
Cl1 O2 1.417(6) . ?
Cl1 O4 1.429(5) . ?
Cl1 O3 1.433(4) . ?
Cl1 O3 1.433(4) 6_565 ?
Cl2 O6 1.431(6) . ?
Cl2 O8 1.436(5) . ?
Cl2 O7 1.445(4) 6_565 ?
Cl2 O7 1.445(4) . ?
