#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/98/2229851.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_2229851
loop_
_publ_author_name
'Czapik, Agnieszka'
'Papadopoulos, Christos'
'Lalia-Kantouri, Maria'
'Gdaniec, Maria'
_publ_section_title
;
 (Carbonato-κ²O,O')bis(di-2-pyridylamine-κ²N,N')cobalt(III)
 bromide
;
_journal_coeditor_code           SU2260
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m414
_journal_page_last               m415
_journal_paper_doi               10.1107/S1600536811008051
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Co (C O3) (C10 H9 N3)2] Br'
_chemical_formula_moiety         'C21 H18 Co N6 O3 +, Br -'
_chemical_formula_sum            'C21 H18 Br Co N6 O3'
_chemical_formula_weight         541.25
_chemical_name_systematic
;(Carbonato-κ²O,O')bis(di-2-pyridylamine-
κ²N,N')cobalt(III) bromide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.839(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9605(3)
_cell_length_b                   7.43220(10)
_cell_length_c                   17.2590(4)
_cell_measurement_reflns_used    8233
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.26
_cell_measurement_theta_min      2.98
_cell_volume                     2092.96(7)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2010)'
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2010)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2010)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and Mercury (Macrae et al.,
2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur E'
_diffrn_measurement_method       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  0.0642
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29846
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    2.767
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Agilent Technologies, 2010)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.499
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0366
_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)+(0.0316P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0800
_reflns_number_gt                3386
_reflns_number_total             4277
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            su2260.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2229851
_cod_database_fobs_code          2229851
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.79115(2) 0.47425(5) 0.48500(2) 0.01679(12) Uani d . 1 . .
Br Br1 0.42522(2) 0.71322(4) 0.36946(2) 0.02940(11) Uani d . 1 . .
N N1A 0.83606(15) 0.3707(3) 0.40419(14) 0.0189(6) Uani d . 1 . .
C C2A 0.91367(19) 0.3175(4) 0.42120(18) 0.0203(7) Uani d . 1 . .
C C3A 0.9525(2) 0.2829(4) 0.36081(19) 0.0255(8) Uani d . 1 . .
H H3A 1.0091 0.2535 0.3741 0.031 Uiso calc R 1 . .
C C4A 0.9066(2) 0.2925(4) 0.2818(2) 0.0305(8) Uani d . 1 . .
H H4A 0.9311 0.2677 0.2396 0.037 Uiso calc R 1 . .
C C5A 0.8242(2) 0.3387(4) 0.2639(2) 0.0303(8) Uani d . 1 . .
H H5A 0.7914 0.3429 0.2097 0.036 Uiso calc R 1 . .
C C6A 0.7916(2) 0.3778(4) 0.32558(18) 0.0261(8) Uani d . 1 . .
H H6A 0.7355 0.4114 0.3134 0.031 Uiso calc R 1 . .
N N7A 0.95794(15) 0.2983(3) 0.50046(15) 0.0223(6) Uani d . 1 . .
H H7A 1.0091 0.2787 0.5059 0.027 Uiso d R 1 . .
C C8A 0.92811(19) 0.2571(4) 0.56488(18) 0.0193(7) Uani d . 1 . .
N N9A 0.85087(15) 0.3025(3) 0.56334(14) 0.0171(6) Uani d . 1 . .
C C10A 0.8212(2) 0.2466(4) 0.62506(18) 0.0211(7) Uani d . 1 . .
H H10A 0.7656 0.2708 0.6227 0.025 Uiso calc R 1 . .
C C11A 0.8687(2) 0.1567(4) 0.69034(19) 0.0253(8) Uani d . 1 . .
H H11A 0.8469 0.1205 0.7331 0.030 Uiso calc R 1 . .
C C12A 0.9494(2) 0.1196(4) 0.6927(2) 0.0287(8) Uani d . 1 . .
H H12A 0.9838 0.0598 0.7381 0.034 Uiso calc R 1 . .
C C13A 0.9796(2) 0.1685(4) 0.63018(19) 0.0266(8) Uani d . 1 . .
H H13A 1.0347 0.1426 0.6313 0.032 Uiso calc R 1 . .
N N1B 0.74231(14) 0.5957(3) 0.55895(14) 0.0169(5) Uani d . 1 . .
C C2B 0.66482(18) 0.6546(4) 0.53146(17) 0.0171(7) Uani d . 1 . .
C C3B 0.63533(19) 0.7949(4) 0.56985(18) 0.0195(7) Uani d . 1 . .
H H3B 0.5827 0.8453 0.5464 0.023 Uiso calc R 1 . .
C C4B 0.68320(19) 0.8582(4) 0.64138(19) 0.0223(7) Uani d . 1 . .
H H4B 0.6641 0.9530 0.6685 0.027 Uiso calc R 1 . .
C C5B 0.76043(19) 0.7830(4) 0.67458(19) 0.0219(7) Uani d . 1 . .
H H5B 0.7926 0.8179 0.7265 0.026 Uiso calc R 1 . .
C C6B 0.78852(19) 0.6586(4) 0.63082(18) 0.0202(7) Uani d . 1 . .
H H6B 0.8427 0.6139 0.6514 0.024 Uiso calc R 1 . .
N N7B 0.61387(15) 0.5775(3) 0.46391(14) 0.0182(6) Uani d . 1 . .
H H7B 0.5646 0.6183 0.4492 0.022 Uiso d R 1 . .
C C8B 0.61995(18) 0.4030(4) 0.43871(17) 0.0173(7) Uani d . 1 . .
N N9B 0.69443(15) 0.3281(3) 0.45216(14) 0.0170(6) Uani d . 1 . .
C C10B 0.69889(19) 0.1502(4) 0.43516(18) 0.0203(7) Uani d . 1 . .
H H10B 0.7512 0.0943 0.4474 0.024 Uiso calc R 1 . .
C C11B 0.63142(19) 0.0493(4) 0.40141(18) 0.0219(7) Uani d . 1 . .
H H11B 0.6365 -0.0754 0.3917 0.026 Uiso calc R 1 . .
C C12B 0.5554(2) 0.1309(4) 0.38152(18) 0.0248(7) Uani d . 1 . .
H H12B 0.5078 0.0643 0.3553 0.030 Uiso calc R 1 . .
C C13B 0.54920(19) 0.3088(4) 0.39994(18) 0.0224(7) Uani d . 1 . .
H H13B 0.4974 0.3670 0.3865 0.027 Uiso calc R 1 . .
C C1 0.82969(19) 0.7580(4) 0.4471(2) 0.0224(7) Uani d . 1 . .
O O1 0.75759(13) 0.6760(3) 0.41586(12) 0.0240(5) Uani d . 1 . .
O O2 0.87502(12) 0.6516(3) 0.50343(12) 0.0229(5) Uani d . 1 . .
O O3 0.85043(14) 0.8971(3) 0.42570(15) 0.0363(6) Uani d . 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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
O2 Co1 O1 . . 68.96(9) y
O2 Co1 N9B . . 169.04(10) y
O1 Co1 N9B . . 100.10(10) y
O2 Co1 N1A . . 88.42(10) y
O1 Co1 N1A . . 88.32(10) y
N9B Co1 N1A . . 92.01(10) y
O2 Co1 N1B . . 90.10(9) y
O1 Co1 N1B . . 86.40(9) y
N9B Co1 N1B . . 88.48(10) y
N1A Co1 N1B . . 174.69(10) y
O2 Co1 N9A . . 96.62(10) y
O1 Co1 N9A . . 165.55(10) y
N9B Co1 N9A . . 94.32(10) y
N1A Co1 N9A . . 90.42(10) y
N1B Co1 N9A . . 94.81(10) y
C2A N1A C6A . . 118.5(3) ?
C2A N1A Co1 . . 121.6(2) ?
C6A N1A Co1 . . 119.1(2) ?
N1A C2A N7A . . 119.3(3) ?
N1A C2A C3A . . 122.0(3) ?
N7A C2A C3A . . 118.7(3) ?
C4A C3A C2A . . 118.3(3) ?
C4A C3A H3A . . 120.9 ?
C2A C3A H3A . . 120.9 ?
C3A C4A C5A . . 119.8(3) ?
C3A C4A H4A . . 120.1 ?
C5A C4A H4A . . 120.1 ?
C6A C5A C4A . . 118.6(3) ?
C6A C5A H5A . . 120.7 ?
C4A C5A H5A . . 120.7 ?
C5A C6A N1A . . 122.6(3) ?
C5A C6A H6A . . 118.7 ?
N1A C6A H6A . . 118.7 ?
C2A N7A C8A . . 127.2(3) ?
C2A N7A H7A . . 112.7 ?
C8A N7A H7A . . 117.3 ?
N9A C8A N7A . . 119.9(3) ?
N9A C8A C13A . . 121.9(3) ?
N7A C8A C13A . . 118.2(3) ?
C8A N9A C10A . . 118.3(3) ?
C8A N9A Co1 . . 120.1(2) ?
C10A N9A Co1 . . 120.9(2) ?
N9A C10A C11A . . 122.2(3) ?
N9A C10A H10A . . 118.9 ?
C11A C10A H10A . . 118.9 ?
C10A C11A C12A . . 118.5(3) ?
C10A C11A H11A . . 120.8 ?
C12A C11A H11A . . 120.8 ?
C13A C12A C11A . . 120.3(3) ?
C13A C12A H12A . . 119.8 ?
C11A C12A H12A . . 119.8 ?
C12A C13A C8A . . 118.7(3) ?
C12A C13A H13A . . 120.7 ?
C8A C13A H13A . . 120.7 ?
C2B N1B C6B . . 118.4(3) ?
C2B N1B Co1 . . 118.4(2) ?
C6B N1B Co1 . . 121.5(2) ?
N1B C2B N7B . . 119.5(3) ?
N1B C2B C3B . . 121.2(3) ?
N7B C2B C3B . . 119.3(3) ?
C4B C3B C2B . . 119.0(3) ?
C4B C3B H3B . . 120.5 ?
C2B C3B H3B . . 120.5 ?
C3B C4B C5B . . 119.6(3) ?
C3B C4B H4B . . 120.2 ?
C5B C4B H4B . . 120.2 ?
C6B C5B C4B . . 118.5(3) ?
C6B C5B H5B . . 120.8 ?
C4B C5B H5B . . 120.8 ?
N1B C6B C5B . . 122.6(3) ?
N1B C6B H6B . . 118.7 ?
C5B C6B H6B . . 118.7 ?
C2B N7B C8B . . 125.2(2) ?
C2B N7B H7B . . 116.0 ?
C8B N7B H7B . . 112.9 ?
N9B C8B N7B . . 118.9(3) ?
N9B C8B C13B . . 121.5(3) ?
N7B C8B C13B . . 119.7(3) ?
C8B N9B C10B . . 118.1(2) ?
C8B N9B Co1 . . 120.32(19) ?
C10B N9B Co1 . . 121.3(2) ?
N9B C10B C11B . . 122.6(3) ?
N9B C10B H10B . . 118.7 ?
C11B C10B H10B . . 118.7 ?
C10B C11B C12B . . 118.9(3) ?
C10B C11B H11B . . 120.5 ?
C12B C11B H11B . . 120.5 ?
C13B C12B C11B . . 119.5(3) ?
C13B C12B H12B . . 120.3 ?
C11B C12B H12B . . 120.3 ?
C12B C13B C8B . . 119.1(3) ?
C12B C13B H13B . . 120.5 ?
C8B C13B H13B . . 120.5 ?
O3 C1 O2 . . 126.0(3) ?
O3 C1 O1 . . 126.0(3) ?
O2 C1 O1 . . 107.9(3) ?
O3 C1 Co1 . . 177.2(3) ?
O2 C1 Co1 . . 53.86(14) ?
O1 C1 Co1 . . 54.00(14) ?
C1 O1 Co1 . . 91.28(17) ?
C1 O2 Co1 . . 91.90(18) ?
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 O2 . 1.901(2) y
Co1 O1 . 1.904(2) y
Co1 N9B . 1.919(2) y
Co1 N1A . 1.923(2) y
Co1 N1B . 1.925(2) y
Co1 N9A . 1.933(2) y
N1A C2A . 1.328(4) ?
N1A C6A . 1.362(4) ?
C2A N7A . 1.376(4) ?
C2A C3A . 1.401(4) ?
C3A C4A . 1.375(4) ?
C3A H3A . 0.9500 ?
C4A C5A . 1.389(5) ?
C4A H4A . 0.9500 ?
C5A C6A . 1.358(4) ?
C5A H5A . 0.9500 ?
C6A H6A . 0.9500 ?
N7A C8A . 1.376(4) ?
N7A H7A . 0.8600 ?
C8A N9A . 1.346(4) ?
C8A C13A . 1.389(4) ?
N9A C10A . 1.362(4) ?
C10A C11A . 1.367(4) ?
C10A H10A . 0.9500 ?
C11A C12A . 1.386(5) ?
C11A H11A . 0.9500 ?
C12A C13A . 1.364(4) ?
C12A H12A . 0.9500 ?
C13A H13A . 0.9500 ?
N1B C2B . 1.343(4) ?
N1B C6B . 1.357(4) ?
C2B N7B . 1.373(4) ?
C2B C3B . 1.399(4) ?
C3B C4B . 1.363(4) ?
C3B H3B . 0.9500 ?
C4B C5B . 1.395(4) ?
C4B H4B . 0.9500 ?
C5B C6B . 1.360(4) ?
C5B H5B . 0.9500 ?
C6B H6B . 0.9500 ?
N7B C8B . 1.380(4) ?
N7B H7B . 0.8599 ?
C8B N9B . 1.341(4) ?
C8B C13B . 1.393(4) ?
N9B C10B . 1.361(4) ?
C10B C11B . 1.359(4) ?
C10B H10B . 0.9500 ?
C11B C12B . 1.380(4) ?
C11B H11B . 0.9500 ?
C12B C13B . 1.371(4) ?
C12B H12B . 0.9500 ?
C13B H13B . 0.9500 ?
C1 O3 . 1.183(4) ?
C1 O2 . 1.325(4) ?
C1 O1 . 1.341(4) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N7A H7A O2 3_766 0.86 2.08 2.876(3) 154
N7B H7B Br1 . 0.86 2.49 3.327(2) 164
C10B H10B O3 1_545 0.95 2.34 3.225(4) 155
C5A H5A O1 2_645 0.95 2.44 3.265(4) 146
C13A H13A O3 3_766 0.95 2.43 3.316(4) 156
C13B H13B Br1 . 0.95 2.83 3.623(3) 142
C5B H5B Br1 4_676 0.95 2.86 3.741(3) 155
C4B H4B Br1 3_676 0.95 2.89 3.657(3) 139
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1A C2A N7A C8A . . . . 28.1(4) ?
N9A C8A N7A C2A . . . . -27.6(4) ?
N1B C2B N7B C8B . . . . 28.0(4) ?
N9B C8B N7B C2B . . . . -33.5(4) ?
