#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:49:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179265 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/85/4318504.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_4318504
loop_
_publ_author_name
'Md. Badruz Zaman'
'Mark D. Smith'
'Delia M. Ciurtin'
'Hans-Conrad zur Loye'
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of South Carolina
Columbia, South Carolina 29208
USA
;
_publ_contact_author_email       zurloye@sc.edu
_publ_contact_author_fax         '803 777 8508'
_publ_contact_author_name        'Professor Hans-Conrad zur Loye'
_publ_contact_author_phone       '803 777 6916'
_publ_section_title
;
 New Cd(II)-, Co(II)-, and Cu(II)-Containing Coordination Polymers
 Synthesized by Using the Rigid Ligand 1,2-Bis(3-pyridyl)ethyne (3,3'-DPA)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4895
_journal_page_last               4903
_journal_paper_doi               10.1021/ic011305x
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C26 H20 Co N6 O10'
_chemical_formula_weight         635.41
_chemical_name_common
;

Co(3-dpa)2(H2O)2(NO3)2 2(MeOH)

;
_chemical_name_systematic
;

?

;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.248(4)
_cell_length_b                   19.982(7)
_cell_length_c                   35.093(16)
_cell_measurement_reflns_used    6079
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.337
_cell_measurement_theta_min      2.327
_cell_volume                     6485(5)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.619 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            10456
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  0.9003
_exptl_absorpt_correction_T_min  0.7514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1660
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0576
_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)+(0.1233P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1700
_reflns_number_gt                1421
_reflns_number_total             1660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011305x_3.cif
_cod_data_source_block           2
_cod_original_cell_volume        6485(4)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4318504
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
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 0.6250 0.6250 0.6250 0.0431(3) Uani 1 4 d S . .
C1 C 0.5295(3) 0.49803(12) 0.58131(7) 0.0512(6) Uani 1 1 d . . .
H1 H 0.4623 0.4958 0.6010 0.061 Uiso 1 1 calc R . .
C2 C 0.5278(3) 0.44857(13) 0.55374(8) 0.0565(7) Uani 1 1 d . . .
C3 C 0.6292(3) 0.45088(18) 0.52457(11) 0.0730(10) Uani 1 1 d . . .
H3 H 0.6304 0.4185 0.5055 0.088 Uiso 1 1 calc R . .
C4 C 0.7282(4) 0.50259(17) 0.52463(10) 0.0730(9) Uani 1 1 d . . .
H4 H 0.7990 0.5049 0.5059 0.088 Uiso 1 1 calc R . .
C5 C 0.7214(3) 0.55032(15) 0.55244(9) 0.0606(7) Uani 1 1 d . . .
H5 H 0.7874 0.5854 0.5517 0.073 Uiso 1 1 calc R . .
C6 C 0.4199(4) 0.39651(16) 0.55473(9) 0.0645(8) Uani 1 1 d . . .
N1 N 0.6239(2) 0.54900(11) 0.58089(7) 0.0492(6) Uani 1 1 d . . .
O1W O 0.8519(3) 0.6250 0.6250 0.0596(7) Uani 1 2 d SD . .
H1W H 0.911(4) 0.646(2) 0.6113(13) 0.112(16) Uiso 1 1 d D . .
N2 N 0.1250 0.6250 0.5537(2) 0.130(3) Uani 1 2 d SD . .
O1 O 0.2403(6) 0.5925(3) 0.5617(2) 0.099(2) Uani 0.50 1 d PD . .
O2 O 0.0478(6) 0.5882(4) 0.5319(2) 0.117(2) Uani 0.50 1 d PD . .
O3 O 0.078(3) 0.6794(6) 0.5636(7) 0.61(4) Uani 0.50 1 d PD . .
C1S C 0.059(6) 0.7790(19) 0.6380(10) 0.41(5) Uani 0.50 1 d PD A -1
O1S O -0.036(3) 0.8364(12) 0.6521(5) 0.41(3) Uani 0.50 1 d PD A -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'
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
O1W Co O1W 180.000(1) 14 . ?
O1W Co N1 89.72(5) 14 8 ?
O1W Co N1 90.28(5) . 8 ?
O1W Co N1 90.28(5) 14 14 ?
O1W Co N1 89.72(5) . 14 ?
N1 Co N1 91.11(13) 8 14 ?
O1W Co N1 89.72(5) 14 . ?
O1W Co N1 90.28(5) . . ?
N1 Co N1 179.44(11) 8 . ?
N1 Co N1 88.90(13) 14 . ?
O1W Co N1 90.28(5) 14 11 ?
O1W Co N1 89.72(5) . 11 ?
N1 Co N1 88.90(13) 8 11 ?
N1 Co N1 179.44(11) 14 11 ?
N1 Co N1 91.11(13) . 11 ?
N1 C1 C2 122.8(2) . . ?
C1 C2 C3 119.0(3) . . ?
C1 C2 C6 120.4(3) . . ?
C3 C2 C6 120.6(3) . . ?
C4 C3 C2 118.1(3) . . ?
C5 C4 C3 119.5(3) . . ?
N1 C5 C4 123.2(3) . . ?
C6 C6 C2 178.6(2) 2 . ?
C1 N1 C5 117.3(2) . . ?
C1 N1 Co 121.80(18) . . ?
C5 N1 Co 120.83(18) . . ?
O3 N2 O3 147(2) . 14_455 ?
O3 N2 O1 35.6(12) . 14_455 ?
O3 N2 O1 133.6(12) 14_455 14_455 ?
O3 N2 O1 133.6(12) . . ?
O3 N2 O1 35.6(12) 14_455 . ?
O1 N2 O1 154.7(9) 14_455 . ?
O3 N2 O2 118.7(11) . . ?
O3 N2 O2 81.8(12) 14_455 . ?
O1 N2 O2 87.6(5) 14_455 . ?
O1 N2 O2 107.7(4) . . ?
O3 N2 O2 81.8(12) . 14_455 ?
O3 N2 O2 118.7(11) 14_455 14_455 ?
O1 N2 O2 107.7(4) 14_455 14_455 ?
O1 N2 O2 87.6(5) . 14_455 ?
O2 N2 O2 106.4(9) . 14_455 ?
O3 O1 N2 68.1(10) 14_455 . ?
O3 O1 O2 109.5(12) 14_455 14_455 ?
N2 O1 O2 46.2(3) . 14_455 ?
N2 O2 O3 47.6(6) . 14_455 ?
N2 O2 O1 46.2(3) . 14_455 ?
O3 O2 O1 84.7(7) 14_455 14_455 ?
O1 O3 N2 76.3(8) 14_455 . ?
O1 O3 O2 113.2(15) 14_455 14_455 ?
N2 O3 O2 50.6(7) . 14_455 ?
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 O1W 2.098(3) 14 ?
Co O1W 2.098(3) . ?
Co N1 2.169(2) 8 ?
Co N1 2.169(2) 14 ?
Co N1 2.169(2) . ?
Co N1 2.169(2) 11 ?
C1 N1 1.341(3) . ?
C1 C2 1.383(4) . ?
C2 C3 1.389(5) . ?
C2 C6 1.442(4) . ?
C3 C4 1.381(4) . ?
C4 C5 1.366(4) . ?
C5 N1 1.346(4) . ?
C6 C6 1.196(6) 2 ?
N2 O3 1.223(8) . ?
N2 O3 1.223(8) 14_455 ?
N2 O1 1.280(5) 14_455 ?
N2 O1 1.280(5) . ?
N2 O2 1.280(6) . ?
N2 O2 1.280(6) 14_455 ?
O1 O3 0.77(2) 14_455 ?
O1 O2 1.772(10) 14_455 ?
O2 O3 1.64(2) 14_455 ?
O2 O1 1.772(10) 14_455 ?
O3 O1 0.77(2) 14_455 ?
O3 O2 1.64(2) 14_455 ?
C1S O1S 1.52(2) . ?
