#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:14:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179805 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/01/7010110.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_7010110
loop_
_publ_author_name
'Ma, Bao-Qing'
'Gao, Song'
'Sun, Hao-Ling'
'Xu, Guang-Xian'
_publ_section_title
;
 Novel three-dimensional networks cross-linked by two sets of hydrogen
 bonded frameworks based on 1-D
 {[M(H2O)4(4,4'-dpdo)][ClO4]2·2(4,4'-dpdo)}n
 (4,4'-dpdo = 4,4'-bipyridine dioxide;
 M = Co, Ni, Cu or Zn)
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              130
_journal_paper_doi               10.1039/b006142p
_journal_year                    2001
_chemical_formula_sum            'C30 H32 Cl2 Co N6 O18'
_chemical_formula_weight         894.45
_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                107.813(2)
_cell_angle_beta                 95.995(2)
_cell_angle_gamma                100.588(2)
_cell_formula_units_Z            1
_cell_length_a                   5.5207(3)
_cell_length_b                   11.8309(5)
_cell_length_c                   14.9809(6)
_cell_measurement_temperature    293(2)
_cell_volume                     902.11(7)
_computing_cell_refinement       'HKL Scalepack'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Denzo $ Maxus'
_computing_molecular_graphics    'Siemens SHELXTL (1990)'
_computing_publication_material  'Siemens SHELXL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.71
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'NONIUS Kappa CCD'
_diffrn_measurement_method       CCD
_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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12296
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   SORTAV
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             459
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0455
_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)+(0.1043P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1628
_reflns_number_gt                3338
_reflns_number_total             4299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006142p.txt
_cod_data_source_block           Codpdo
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P-1
_cod_database_code               7010110
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
Cl1 Cl -0.32591(15) 0.62042(7) 0.29428(6) 0.0484(2) Uani 1 1 d . . .
Co1 Co 0.0000 0.0000 0.0000 0.02320(17) Uani 1 2 d S . .
O1 O -0.2511(3) -0.11723(16) 0.04846(14) 0.0309(4) Uani 1 1 d . . .
O2 O 0.1108(4) 0.0691(3) 0.30266(17) 0.0574(7) Uani 1 1 d . . .
O3 O -0.3448(4) 0.1801(3) 0.19922(16) 0.0617(8) Uani 1 1 d . . .
O4 O 0.1658(4) 0.0961(2) 0.13844(14) 0.0404(5) Uani 1 1 d . . .
H2 H 0.110(7) 0.069(4) 0.191(3) 0.063(11) Uiso 1 1 d . . .
H1 H 0.335(8) 0.121(3) 0.167(3) 0.053(10) Uiso 1 1 d . . .
O5 O -0.2506(4) 0.11711(18) 0.02372(16) 0.0329(5) Uani 1 1 d . . .
H4 H -0.369(6) 0.112(3) -0.002(2) 0.025(8) Uiso 1 1 d . . .
H3 H -0.277(7) 0.156(3) 0.096(3) 0.056(10) Uiso 1 1 d . . .
O6 O -0.4181(6) 0.4912(2) 0.2547(2) 0.0777(9) Uani 1 1 d . . .
O7 O -0.0618(5) 0.6551(3) 0.3025(2) 0.0835(10) Uani 1 1 d . . .
O8 O -0.4391(6) 0.6768(2) 0.2336(2) 0.0682(8) Uani 1 1 d . . .
O9 O -0.3895(7) 0.6610(3) 0.3866(2) 0.0900(11) Uani 1 1 d . . .
N1 N -0.1924(4) -0.22543(19) 0.03685(16) 0.0284(5) Uani 1 1 d . . .
N2 N -0.0617(5) 0.0539(2) 0.35482(18) 0.0400(6) Uani 1 1 d . . .
N3 N -0.2491(4) 0.2675(2) 0.28186(16) 0.0372(6) Uani 1 1 d . . .
C1 C -0.0231(6) -0.2356(3) 0.1036(2) 0.0374(6) Uani 1 1 d . . .
H1A H 0.0433 -0.1695 0.1588 0.045 Uiso 1 1 calc R . .
C2 C 0.0520(6) -0.3426(3) 0.0906(2) 0.0385(7) Uani 1 1 d . . .
H2A H 0.1675 -0.3489 0.1377 0.046 Uiso 1 1 calc R . .
C3 C -0.0415(5) -0.4417(2) 0.0085(2) 0.0316(6) Uani 1 1 d . . .
C4 C -0.2221(7) -0.4281(3) -0.0566(3) 0.0513(9) Uani 1 1 d . . .
H4A H -0.2957 -0.4938 -0.1113 0.062 Uiso 1 1 calc R . .
C5 C -0.2944(6) -0.3202(3) -0.0422(2) 0.0451(8) Uani 1 1 d . . .
H5A H -0.4142 -0.3128 -0.0872 0.054 Uiso 1 1 calc R . .
C6 C -0.2731(6) -0.0331(3) 0.3176(2) 0.0478(8) Uani 1 1 d . . .
H6A H -0.3031 -0.0789 0.2533 0.057 Uiso 1 1 calc R . .
C7 C -0.4445(6) -0.0550(3) 0.3733(2) 0.0455(8) Uani 1 1 d . . .
H7A H -0.5877 -0.1169 0.3464 0.055 Uiso 1 1 calc R . .
C8 C -0.4093(5) 0.0133(3) 0.4692(2) 0.0339(6) Uani 1 1 d . . .
C9 C -0.1952(6) 0.1062(3) 0.5038(2) 0.0438(7) Uani 1 1 d . . .
H9A H -0.1674 0.1569 0.5669 0.053 Uiso 1 1 calc R . .
C10 C -0.0241(6) 0.1248(3) 0.4470(2) 0.0449(7) Uani 1 1 d . . .
H10A H 0.1196 0.1869 0.4722 0.054 Uiso 1 1 calc R . .
C11 C -0.3778(6) 0.2803(3) 0.3541(2) 0.0400(7) Uani 1 1 d . . .
H11A H -0.5319 0.2276 0.3461 0.048 Uiso 1 1 calc R . .
C12 C -0.2827(5) 0.3707(3) 0.4394(2) 0.0373(7) Uani 1 1 d . . .
H12A H -0.3745 0.3792 0.4887 0.045 Uiso 1 1 calc R . .
C13 C -0.0518(5) 0.4503(2) 0.45392(19) 0.0301(6) Uani 1 1 d . . .
C14 C 0.0763(5) 0.4325(3) 0.3768(2) 0.0379(7) Uani 1 1 d . . .
H14A H 0.2321 0.4829 0.3830 0.046 Uiso 1 1 calc R . .
C15 C -0.0255(5) 0.3419(3) 0.2926(2) 0.0409(7) Uani 1 1 d . . .
H15A H 0.0614 0.3317 0.2418 0.049 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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
O7 Cl1 O9 108.6(2) . . ?
O7 Cl1 O6 112.1(2) . . ?
O9 Cl1 O6 108.4(2) . . ?
O7 Cl1 O8 108.4(2) . . ?
O9 Cl1 O8 110.3(2) . . ?
O6 Cl1 O8 108.94(17) . . ?
O4 Co1 O4 180.00(12) 2 . ?
O4 Co1 O5 94.81(9) 2 . ?
O4 Co1 O5 85.19(9) . . ?
O4 Co1 O5 85.19(9) 2 2 ?
O4 Co1 O5 94.81(9) . 2 ?
O5 Co1 O5 180.00(15) . 2 ?
O4 Co1 O1 90.55(8) 2 . ?
O4 Co1 O1 89.45(8) . . ?
O5 Co1 O1 86.74(7) . . ?
O5 Co1 O1 93.26(7) 2 . ?
O4 Co1 O1 89.45(8) 2 2 ?
O4 Co1 O1 90.55(8) . 2 ?
O5 Co1 O1 93.26(7) . 2 ?
O5 Co1 O1 86.74(7) 2 2 ?
O1 Co1 O1 180.00(10) . 2 ?
N1 O1 Co1 113.12(13) . . ?
C5 N1 O1 120.1(2) . . ?
C5 N1 C1 120.8(2) . . ?
O1 N1 C1 119.1(2) . . ?
O2 N2 C6 120.6(3) . . ?
O2 N2 C10 119.8(3) . . ?
C6 N2 C10 119.7(3) . . ?
O3 N3 C11 119.4(2) . . ?
O3 N3 C15 120.0(2) . . ?
C11 N3 C15 120.6(2) . . ?
N1 C1 C2 120.3(3) . . ?
C1 C2 C3 121.0(3) . . ?
C2 C3 C4 116.5(3) . . ?
C2 C3 C3 122.1(3) . 2_545 ?
C4 C3 C3 121.4(3) . 2_545 ?
C5 C4 C3 121.5(3) . . ?
N1 C5 C4 119.9(3) . . ?
N2 C6 C7 120.7(3) . . ?
C6 C7 C8 121.4(3) . . ?
C9 C8 C7 116.1(3) . . ?
C9 C8 C8 122.3(3) . 2_456 ?
C7 C8 C8 121.5(3) . 2_456 ?
C10 C9 C8 121.3(3) . . ?
N2 C10 C9 120.7(3) . . ?
N3 C11 C12 120.1(3) . . ?
C11 C12 C13 121.4(3) . . ?
C12 C13 C14 116.4(2) . . ?
C12 C13 C13 121.8(3) . 2_566 ?
C14 C13 C13 121.8(3) . 2_566 ?
C15 C14 C13 120.5(3) . . ?
N3 C15 C14 121.0(2) . . ?
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
Cl1 O7 1.422(3) . ?
Cl1 O9 1.423(3) . ?
Cl1 O6 1.430(3) . ?
Cl1 O8 1.438(3) . ?
Co1 O4 2.052(2) 2 ?
Co1 O4 2.052(2) . ?
Co1 O5 2.1133(19) . ?
Co1 O5 2.1133(19) 2 ?
Co1 O1 2.1195(18) . ?
Co1 O1 2.1195(18) 2 ?
O1 N1 1.342(3) . ?
O2 N2 1.315(3) . ?
O3 N3 1.327(3) . ?
N1 C5 1.339(4) . ?
N1 C1 1.344(4) . ?
N2 C6 1.343(4) . ?
N2 C10 1.350(4) . ?
N3 C11 1.341(4) . ?
N3 C15 1.341(4) . ?
C1 C2 1.368(4) . ?
C2 C3 1.384(4) . ?
C3 C4 1.386(4) . ?
C3 C3 1.491(5) 2_545 ?
C4 C5 1.368(4) . ?
C6 C7 1.365(5) . ?
C7 C8 1.389(4) . ?
C8 C9 1.386(4) . ?
C8 C8 1.485(5) 2_456 ?
C9 C10 1.367(4) . ?
C11 C12 1.368(4) . ?
C12 C13 1.391(4) . ?
C13 C14 1.399(4) . ?
C13 C13 1.487(5) 2_566 ?
C14 C15 1.363(4) . ?
