#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:09:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179233 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/53/4315305.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_4315305
loop_
_publ_author_name
'Simon M. Humphrey'
'Richard A. Mole'
'Richard I. Thompson'
'Paul T. Wood'
_publ_section_title
;
 Mixed Alkali Metal/Transition Metal Coordination Polymers with the
 Mellitic Acid Hexaanion: 2-Dimensional Hexagonal Magnetic Nets
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3441
_journal_page_last               3448
_journal_paper_doi               10.1021/ic902527e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C12 H4 Co2 O14, 2(H4 N)'
_chemical_formula_sum            'C12 H12 Co2 N2 O14'
_chemical_formula_weight         526.10
_chemical_name_common            'Diammonium dicobalt(II)aquo mellitate'
_chemical_name_systematic
; 
 ? 
;
_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                 116.383(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4267(2)
_cell_length_b                   10.9735(4)
_cell_length_c                   9.0131(3)
_cell_measurement_reflns_used    3767
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.02
_cell_volume                     746.64(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5219
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    2.320
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0320
_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)+(0.0171P)²+1.8353P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                1118
_reflns_number_total             1284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902527e_si_002_3.cif
_cod_data_source_block           pw0901
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4315305
loop_
_publ_contact_author
'Dr. Simon M. Humphrey'
'Dr. Paul T. Wood'
loop_
_publ_contact_author_email
smh@cm.utexas.edu
ptw22@cam.ac.uk
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_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
Co1 Co 1.23254(5) 0.90064(4) 0.81303(5) 0.01120(15) Uani 1 1 d . . .
N1 N 0.0167(4) 0.8240(3) 0.1434(4) 0.0229(7) Uani 1 1 d . . .
H4N H -0.0416 0.8050 0.0291 0.034 Uiso 1 1 d . . .
H3N H 0.1323 0.7918 0.2008 0.034 Uiso 1 1 d . . .
H2N H 0.0190 0.9108 0.1470 0.034 Uiso 1 1 d . . .
H1N H -0.0625 0.7882 0.1806 0.034 Uiso 1 1 d . . .
O1 O 0.9631(3) 0.9336(2) 0.7195(3) 0.0211(6) Uani 1 1 d . . .
O2 O 0.8303(3) 0.7937(2) 0.8071(3) 0.0262(6) Uani 1 1 d . . .
O3 O 0.7269(3) 1.0297(2) 0.9528(3) 0.0153(5) Uani 1 1 d . . .
O4 O 0.5055(3) 0.8960(2) 0.8903(3) 0.0138(5) Uani 1 1 d . . .
O5 O 0.2297(3) 1.0768(2) 0.7256(3) 0.0180(5) Uani 1 1 d . . .
O6 O 0.2615(3) 1.2336(2) 0.5844(3) 0.0169(5) Uani 1 1 d . . .
O7 O 1.1674(3) 0.8221(2) 0.5716(3) 0.0224(6) Uani 1 1 d . . .
H7B H 1.1249 0.7413 0.5426 0.034 Uiso 1 1 d . . .
H7A H 1.0997 0.8829 0.4948 0.034 Uiso 1 1 d . . .
C1 C 0.6538(4) 0.9386(3) 0.6040(4) 0.0112(7) Uani 1 1 d . . .
C2 C 0.5444(4) 0.9882(3) 0.6697(4) 0.0110(7) Uani 1 1 d . . .
C3 C 0.3923(4) 1.0507(3) 0.5645(4) 0.0103(7) Uani 1 1 d . . .
C4 C 0.8287(4) 0.8809(3) 0.7191(4) 0.0149(7) Uani 1 1 d . . .
C5 C 0.5958(4) 0.9713(3) 0.8530(4) 0.0121(7) Uani 1 1 d . . .
C6 C 0.2854(4) 1.1244(3) 0.6310(4) 0.0116(7) Uani 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'
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'
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
O6 Co1 O1 98.20(10) 2_646 . ?
O6 Co1 O5 175.64(9) 2_646 1_655 ?
O1 Co1 O5 81.83(10) . 1_655 ?
O6 Co1 O4 91.45(9) 2_646 1_655 ?
O1 Co1 O4 170.35(10) . 1_655 ?
O5 Co1 O4 88.54(9) 1_655 1_655 ?
O6 Co1 O3 84.96(9) 2_646 3_777 ?
O1 Co1 O3 90.27(9) . 3_777 ?
O5 Co1 O3 90.68(9) 1_655 3_777 ?
O4 Co1 O3 90.58(8) 1_655 3_777 ?
O6 Co1 O7 92.41(9) 2_646 . ?
O1 Co1 O7 85.32(9) . . ?
O5 Co1 O7 91.94(9) 1_655 . ?
O4 Co1 O7 94.31(9) 1_655 . ?
O3 Co1 O7 174.51(9) 3_777 . ?
H4N N1 H3N 115.0 . . ?
H4N N1 H2N 104.5 . . ?
H3N N1 H2N 110.8 . . ?
H4N N1 H1N 100.7 . . ?
H3N N1 H1N 111.4 . . ?
H2N N1 H1N 114.0 . . ?
C4 O1 Co1 137.4(2) . . ?
C5 O3 Co1 126.93(19) . 3_777 ?
C5 O4 Co1 126.8(2) . 1_455 ?
C6 O5 Co1 134.2(2) . 1_455 ?
C6 O6 Co1 137.4(2) . 2_656 ?
Co1 O7 H7B 122.9 . . ?
Co1 O7 H7A 104.8 . . ?
H7B O7 H7A 115.2 . . ?
C3 C1 C2 120.5(3) 3_676 . ?
C3 C1 C4 119.8(3) 3_676 . ?
C2 C1 C4 119.6(3) . . ?
C3 C2 C1 118.8(3) . . ?
C3 C2 C5 122.2(3) . . ?
C1 C2 C5 119.0(3) . . ?
C2 C3 C1 120.7(3) . 3_676 ?
C2 C3 C6 121.5(3) . . ?
C1 C3 C6 117.3(3) 3_676 . ?
O2 C4 O1 126.4(3) . . ?
O2 C4 C1 119.5(3) . . ?
O1 C4 C1 114.0(3) . . ?
O3 C5 O4 126.0(3) . . ?
O3 C5 C2 117.0(3) . . ?
O4 C5 C2 117.0(3) . . ?
O5 C6 O6 124.8(3) . . ?
O5 C6 C3 120.9(3) . . ?
O6 C6 C3 114.3(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
Co1 O6 2.043(2) 2_646 ?
Co1 O1 2.073(2) . ?
Co1 O5 2.084(2) 1_655 ?
Co1 O4 2.087(2) 1_655 ?
Co1 O3 2.125(2) 3_777 ?
Co1 O7 2.172(2) . ?
N1 H4N 0.9471 . ?
N1 H3N 0.9456 . ?
N1 H2N 0.9530 . ?
N1 H1N 0.9543 . ?
O1 C4 1.270(4) . ?
O2 C4 1.240(4) . ?
O3 C5 1.248(4) . ?
O3 Co1 2.125(2) 3_777 ?
O4 C5 1.266(4) . ?
O4 Co1 2.087(2) 1_455 ?
O5 C6 1.255(4) . ?
O5 Co1 2.084(2) 1_455 ?
O6 C6 1.257(4) . ?
O6 Co1 2.043(2) 2_656 ?
O7 H7B 0.9490 . ?
O7 H7A 0.9475 . ?
C1 C3 1.396(4) 3_676 ?
C1 C2 1.408(4) . ?
C1 C4 1.513(5) . ?
C2 C3 1.390(5) . ?
C2 C5 1.522(4) . ?
C3 C1 1.396(4) 3_676 ?
C3 C6 1.518(4) . ?
