#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:38:37 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180347 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/16/7201617.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_7201617
loop_
_publ_author_name
'Braverman, Maxwell A.'
'LaDuca, Robert L.'
_publ_section_title
;
 Hydrothermal synthesis of divalent metal pyromellitate/dipyridylamine
 complexes: From an unprecedented supramolecular three-dimensional
 topology to an anionic coordination polymer framework with large
 incipient cation-bearing voids
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              117
_journal_paper_doi               10.1039/b712182b
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C30 H30 Co N6 O12'
_chemical_formula_weight         725.53
_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                 108.032(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.268(3)
_cell_length_b                   20.930(8)
_cell_length_c                   10.365(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1499.3(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.940
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16275
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             750
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3423
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0347
_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)+(0.0351P)²+1.2801P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                3051
_reflns_number_total             3423
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b712182b.txt
_cod_data_source_block           mono1
_cod_original_cell_volume        1499.2(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7201617
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 0.5000 0.0000 0.5000 0.02100(10) Uani 1 2 d S . .
O1 O 0.7784(2) 0.01384(9) 0.52329(15) 0.0449(4) Uani 1 1 d D . .
H1A H 0.808(4) 0.0154(13) 0.450(2) 0.054 Uiso 1 1 d D . .
H1B H 0.868(3) -0.0023(12) 0.585(2) 0.054 Uiso 1 1 d D . .
O2 O 0.4350(2) 0.06299(7) 0.32612(13) 0.0321(3) Uani 1 1 d D . .
H2A H 0.506(3) 0.0689(11) 0.276(2) 0.038 Uiso 1 1 d D . .
H2B H 0.333(3) 0.0838(10) 0.294(2) 0.038 Uiso 1 1 d D . .
O3 O 0.8861(2) 0.01815(10) 0.31148(14) 0.0561(5) Uani 1 1 d . . .
O4 O 0.6684(2) 0.07567(7) 0.16250(15) 0.0413(4) Uani 1 1 d . . .
O5 O 1.1033(2) 0.14224(6) 0.21273(13) 0.0375(3) Uani 1 1 d . . .
O6 O 1.0563(3) 0.17407(6) 0.00044(14) 0.0443(4) Uani 1 1 d . . .
N1 N 0.5206(2) 0.08210(7) 0.63679(15) 0.0289(3) Uani 1 1 d . . .
N2 N 0.5410(3) 0.30712(8) 1.24277(16) 0.0363(4) Uani 1 1 d D . .
H2N H 0.543(3) 0.3178(11) 1.3263(18) 0.044 Uiso 1 1 d D . .
N3 N 0.5613(3) 0.25037(7) 0.86619(15) 0.0299(3) Uani 1 1 d D . .
H3N H 0.563(3) 0.2832(9) 0.815(2) 0.036 Uiso 1 1 d D . .
C1 C 0.5305(3) 0.14096(9) 0.5892(2) 0.0372(5) Uani 1 1 d . . .
H1 H 0.5265 0.1450 0.4990 0.045 Uiso 1 1 calc R . .
C2 C 0.5461(3) 0.19565(9) 0.66410(19) 0.0363(5) Uani 1 1 d . . .
H2 H 0.5525 0.2351 0.6246 0.044 Uiso 1 1 calc R . .
C3 C 0.5523(3) 0.19217(8) 0.79935(17) 0.0253(3) Uani 1 1 d . . .
C4 C 0.5462(3) 0.13137(9) 0.85142(19) 0.0366(5) Uani 1 1 d . . .
H4 H 0.5522 0.1259 0.9417 0.044 Uiso 1 1 calc R . .
C5 C 0.5310(3) 0.07901(9) 0.76729(19) 0.0361(4) Uani 1 1 d . . .
H5 H 0.5279 0.0387 0.8045 0.043 Uiso 1 1 calc R . .
C6 C 0.5290(3) 0.34951(10) 1.1442(2) 0.0401(5) Uani 1 1 d . . .
H6 H 0.5171 0.3927 1.1610 0.048 Uiso 1 1 calc R . .
C7 C 0.5338(3) 0.33063(9) 1.01970(19) 0.0365(5) Uani 1 1 d . . .
H7 H 0.5235 0.3609 0.9521 0.044 Uiso 1 1 calc R . .
C8 C 0.5542(3) 0.26567(8) 0.99258(18) 0.0267(4) Uani 1 1 d . . .
C9 C 0.5683(4) 0.22271(10) 1.0988(2) 0.0430(5) Uani 1 1 d . . .
H9 H 0.5826 0.1792 1.0863 0.052 Uiso 1 1 calc R . .
C10 C 0.5609(4) 0.24518(10) 1.2207(2) 0.0455(6) Uani 1 1 d . . .
H10 H 0.5700 0.2163 1.2906 0.055 Uiso 1 1 calc R . .
C11 C 0.9138(2) 0.02310(8) 0.09420(16) 0.0222(3) Uani 1 1 d . . .
C12 C 1.0233(2) 0.06403(8) 0.04116(16) 0.0226(3) Uani 1 1 d . . .
C13 C 0.8921(3) -0.04038(8) 0.05215(17) 0.0241(3) Uani 1 1 d . . .
H13 H 0.8189 -0.0677 0.0875 0.029 Uiso 1 1 calc R . .
C15 C 0.8152(3) 0.04272(8) 0.19676(17) 0.0247(3) Uani 1 1 d . . .
C16 C 1.0617(3) 0.13253(8) 0.08750(18) 0.0261(4) 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'
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'
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 Co1 O1 180.00(11) . 3_656 ?
O1 Co1 O2 92.07(6) . 3_656 ?
O1 Co1 O2 87.93(6) 3_656 3_656 ?
O1 Co1 O2 87.93(6) . . ?
O1 Co1 O2 92.07(6) 3_656 . ?
O2 Co1 O2 180.0 3_656 . ?
O1 Co1 N1 86.81(7) . . ?
O1 Co1 N1 93.19(7) 3_656 . ?
O2 Co1 N1 89.16(6) 3_656 . ?
O2 Co1 N1 90.84(6) . . ?
O1 Co1 N1 93.19(7) . 3_656 ?
O1 Co1 N1 86.81(7) 3_656 3_656 ?
O2 Co1 N1 90.84(6) 3_656 3_656 ?
O2 Co1 N1 89.16(6) . 3_656 ?
N1 Co1 N1 180.00(5) . 3_656 ?
C5 N1 C1 115.24(16) . . ?
C5 N1 Co1 125.90(13) . . ?
C1 N1 Co1 118.82(12) . . ?
C10 N2 C6 119.99(17) . . ?
C8 N3 C3 132.26(15) . . ?
N1 C1 C2 124.49(17) . . ?
C1 C2 C3 119.96(17) . . ?
C4 C3 C2 116.42(16) . . ?
C4 C3 N3 127.63(16) . . ?
C2 C3 N3 115.95(16) . . ?
C5 C4 C3 119.14(17) . . ?
N1 C5 C4 124.72(18) . . ?
N2 C6 C7 121.19(18) . . ?
C6 C7 C8 120.40(18) . . ?
N3 C8 C9 126.05(17) . . ?
N3 C8 C7 117.16(16) . . ?
C9 C8 C7 116.78(17) . . ?
C10 C9 C8 119.48(19) . . ?
N2 C10 C9 122.14(19) . . ?
C13 C11 C12 119.11(15) . . ?
C13 C11 C15 116.57(15) . . ?
C12 C11 C15 124.31(16) . . ?
C13 C12 C11 119.09(16) 3_755 . ?
C13 C12 C16 118.80(15) 3_755 . ?
C11 C12 C16 122.03(15) . . ?
C12 C13 C11 121.80(15) 3_755 . ?
O4 C15 O3 124.84(16) . . ?
O4 C15 C11 120.55(15) . . ?
O3 C15 C11 114.33(16) . . ?
O6 C16 O5 125.47(17) . . ?
O6 C16 C12 118.11(15) . . ?
O5 C16 C12 116.37(15) . . ?
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 O1 1.9835(16) . ?
Co1 O1 1.9835(16) 3_656 ?
Co1 O2 2.1638(14) 3_656 ?
Co1 O2 2.1638(14) . ?
Co1 N1 2.2032(16) . ?
Co1 N1 2.2032(16) 3_656 ?
O3 C15 1.251(2) . ?
O4 C15 1.227(2) . ?
O5 C16 1.255(2) . ?
O6 C16 1.245(2) . ?
N1 C5 1.333(2) . ?
N1 C1 1.337(2) . ?
N2 C10 1.332(3) . ?
N2 C6 1.335(3) . ?
N3 C8 1.365(2) . ?
N3 C3 1.393(2) . ?
C1 C2 1.368(3) . ?
C2 C3 1.390(3) . ?
C3 C4 1.388(3) . ?
C4 C5 1.384(3) . ?
C6 C7 1.360(3) . ?
C7 C8 1.405(3) . ?
C8 C9 1.400(3) . ?
C9 C10 1.365(3) . ?
C11 C13 1.392(2) . ?
C11 C12 1.393(2) . ?
C11 C15 1.511(2) . ?
C12 C13 1.388(2) 3_755 ?
C12 C16 1.510(2) . ?
C13 C12 1.388(2) 3_755 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O3 0.849(17) 1.703(17) 2.550(2) 175(3) .
O1 H1B O3 0.829(16) 1.808(19) 2.597(2) 158(3) 3_756
O2 H2A O4 0.842(16) 1.917(16) 2.758(2) 176(2) .
O2 H2B O5 0.836(15) 2.030(16) 2.862(2) 173(2) 1_455
N2 H2N O6 0.890(16) 1.786(17) 2.668(2) 171(2) 4_567
N3 H3N O5 0.872(16) 1.957(16) 2.824(2) 172(2) 4_566
