#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/63/2016308.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_2016308
loop_
_publ_author_name
'Ma, Yi'
'Zhang, Li-Tian'
'Wang, Xiao-Fang'
'He, Yong-Ke'
'Han, Zheng-Bo'
_publ_section_title
;
 A one-dimensional nickel(II) coordination polymer containing
 2,6-dipicolinate and dipyrido[3,2-a:2',3'-c]phenazine
;
_journal_coeditor_code           DN3067
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m573
_journal_page_last               m575
_journal_paper_doi               10.1107/S0108270107053851
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni (C7 H3 N O4) (C18 H10 N4)]'
_chemical_formula_moiety         'C25 H13 N5 Ni O4'
_chemical_formula_sum            'C25 H13 N5 Ni O4'
_chemical_formula_weight         506.11
_chemical_name_systematic
;
catena-poly[(dipyrido[3,2-a:2',3'-c]phenazine-κ²N,N')nickel(II)]-μ-\
2,6-dipicolinato-κ³O²,O⁶:O^2'^]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 106.906(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3482(11)
_cell_length_b                   35.825(4)
_cell_length_c                   7.8986(12)
_cell_measurement_reflns_used    3623
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      2.35
_cell_volume                     1989.4(5)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia,
1997)
and PLATON (Spek, 2003)
;
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX area-detector diffractometer'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4459
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  0.7795
_exptl_absorpt_correction_T_min  0.7037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'(SADABS; Sheldrick, 1996)'
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.600
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3504
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0401
_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)+(0.0536P)²+1.7276P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                2860
_reflns_number_total             3504
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn3067.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2016308
_cod_database_fobs_code          2016308
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ni Ni1 0.82244(5) 0.185119(10) 0.64973(5) 0.02248(15) Uani d . 1
C C1 0.8131(4) 0.25886(9) 0.4786(4) 0.0245(7) Uani d . 1
C C2 0.6213(4) 0.24791(9) 0.4585(4) 0.0244(7) Uani d . 1
C C3 0.4735(5) 0.27022(10) 0.3964(5) 0.0311(8) Uani d . 1
H H3A 0.4856 0.2952 0.3690 0.037 Uiso calc R 1
C C4 0.3081(5) 0.25400(11) 0.3767(5) 0.0386(9) Uani d . 1
H H4A 0.1971 0.2678 0.3336 0.046 Uiso calc R 1
C C5 0.2962(5) 0.21686(11) 0.4191(5) 0.0361(9) Uani d . 1
H H5A 0.1771 0.2058 0.3971 0.043 Uiso calc R 1
C C6 0.4508(4) 0.19662(9) 0.4903(4) 0.0255(7) Uani d . 1
C C7 0.4676(5) 0.15682(9) 0.5624(4) 0.0278(7) Uani d . 1
C C8 1.1226(5) 0.15194(10) 0.9717(5) 0.0320(8) Uani d . 1
H H8A 1.1054 0.1726 1.0368 0.038 Uiso calc R 1
C C9 1.2380(5) 0.12336(11) 1.0570(5) 0.0399(9) Uani d . 1
H H9A 1.3003 0.1241 1.1777 0.048 Uiso calc R 1
C C10 1.2557(5) 0.09312(10) 0.9510(5) 0.0368(9) Uani d . 1
H H10A 1.3311 0.0731 1.0051 0.044 Uiso calc R 1
C C11 1.1607(4) 0.09087(8) 0.7554(4) 0.0271(7) Uani d D 1
C C12 1.1744(4) 0.06117(9) 0.6383(5) 0.0284(7) Uani d D 1
C C13 1.2856(5) 0.00363(9) 0.5917(6) 0.0360(9) Uani d . 1
C C14 1.3943(5) -0.02765(10) 0.6627(6) 0.0451(10) Uani d . 1
H H14A 1.4562 -0.0296 0.7831 0.054 Uiso calc R 1
C C15 1.4053(6) -0.05583(11) 0.5437(7) 0.0518(12) Uani d . 1
H H15A 1.4778 -0.0768 0.5897 0.062 Uiso calc R 1
C C16 1.3118(6) -0.05511(11) 0.3517(7) 0.0515(11) Uani d . 1
H H16A 1.3262 -0.0751 0.2818 0.062 Uiso calc R 1
C C17 1.2049(6) -0.02541(11) 0.2768(7) 0.0490(11) Uani d . 1
H H17A 1.1439 -0.0243 0.1559 0.059 Uiso calc R 1
C C18 1.1903(5) 0.00476(10) 0.3955(6) 0.0376(9) Uani d . 1
C C19 1.0778(4) 0.06153(9) 0.4384(5) 0.0281(7) Uani d . 1
C C20 0.9642(4) 0.09347(9) 0.3624(5) 0.0264(7) Uani d . 1
C C21 0.8637(5) 0.09625(11) 0.1724(5) 0.0352(8) Uani d . 1
H H21A 0.8718 0.0771 0.0955 0.042 Uiso calc R 1
C C22 0.7602(5) 0.12692(11) 0.1118(5) 0.0374(9) Uani d . 1
H H22A 0.6959 0.1302 -0.0075 0.045 Uiso calc R 1
C C23 0.7549(5) 0.15433(10) 0.2423(5) 0.0335(8) Uani d . 1
H H23A 0.6824 0.1755 0.2018 0.040 Uiso calc R 1
C C24 0.9509(4) 0.12229(9) 0.4840(4) 0.0225(7) Uani d . 1
C C25 1.0507(4) 0.12140(8) 0.6841(4) 0.0231(7) Uani d D 1
N N1 0.6076(3) 0.21282(7) 0.5092(4) 0.0223(6) Uani d . 1
N N2 1.0299(4) 0.15092(7) 0.7891(4) 0.0249(6) Uani d . 1
N N3 0.8472(4) 0.15269(7) 0.4247(4) 0.0257(6) Uani d . 1
N N4 1.2762(4) 0.03168(8) 0.7101(4) 0.0336(7) Uani d . 1
N N5 1.0869(4) 0.03420(8) 0.3203(4) 0.0346(7) Uani d . 1
O O1 0.8402(3) 0.28967(6) 0.4126(3) 0.0339(6) Uani d . 1
O O2 0.9272(3) 0.23526(6) 0.5597(3) 0.0331(6) Uani d . 1
O O3 0.3351(3) 0.13674(7) 0.5182(4) 0.0450(7) Uani d . 1
O O4 0.6220(3) 0.14774(6) 0.6653(3) 0.0308(5) 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'
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'
Ni Ni 0.3393 1.1124 '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_3
_geom_angle
_geom_angle_publ_flag
N1 Ni1 N2 . 173.60(11) yes
N1 Ni1 O4 . 83.48(10) yes
N2 Ni1 O4 . 90.72(10) yes
N1 Ni1 O2 . 72.01(9) yes
N2 Ni1 O2 . 113.65(10) yes
O4 Ni1 O2 . 155.40(9) yes
N1 Ni1 N3 . 93.08(11) ?
N2 Ni1 N3 . 83.80(10) ?
O4 Ni1 N3 . 86.07(10) ?
O2 Ni1 N3 . 93.01(10) ?
N1 Ni1 O1 4_566 98.30(10) ?
N2 Ni1 O1 4_566 84.69(10) ?
O4 Ni1 O1 4_566 93.33(10) ?
O2 Ni1 O1 4_566 92.29(9) yes
N3 Ni1 O1 4_566 168.47(9) ?
O2 C1 O1 . 130.6(3) ?
O2 C1 C2 . 111.8(3) ?
O1 C1 C2 . 117.7(3) ?
C3 C2 N1 . 123.8(3) ?
C3 C2 C1 . 123.6(3) ?
N1 C2 C1 . 112.6(3) ?
C4 C3 C2 . 114.1(3) ?
C4 C3 H3A . 123.0 ?
C2 C3 H3A . 123.0 ?
C3 C4 C5 . 121.2(3) ?
C3 C4 H4A . 119.4 ?
C5 C4 H4A . 119.4 ?
C6 C5 C4 . 121.5(3) ?
C6 C5 H5A . 119.3 ?
C4 C5 H5A . 119.3 ?
N1 C6 C5 . 116.0(3) ?
N1 C6 C7 . 114.5(3) ?
C5 C6 C7 . 129.4(3) ?
O3 C7 O4 . 123.9(3) ?
O3 C7 C6 . 119.3(3) ?
O4 C7 C6 . 116.9(3) ?
C9 C8 N2 . 122.0(3) ?
C9 C8 H8A . 119.0 ?
N2 C8 H8A . 119.0 ?
C8 C9 C10 . 115.8(3) ?
C8 C9 H9A . 122.1 ?
C10 C9 H9A . 122.1 ?
C9 C10 C11 . 124.2(3) ?
C9 C10 H10A . 117.9 ?
C11 C10 H10A . 117.9 ?
C25 C11 C10 . 114.8(3) ?
C25 C11 C12 . 118.0(3) ?
C10 C11 C12 . 127.3(3) ?
N4 C12 C11 . 117.0(3) ?
N4 C12 C19 . 118.9(3) ?
C11 C12 C19 . 124.1(3) ?
N4 C13 C14 . 116.5(4) ?
N4 C13 C18 . 125.1(3) ?
C14 C13 C18 . 118.4(3) ?
C13 C14 C15 . 116.7(4) ?
C13 C14 H14A . 121.7 ?
C15 C14 H14A . 121.7 ?
C14 C15 C16 . 125.4(4) ?
C14 C15 H15A . 117.3 ?
C16 C15 H15A . 117.3 ?
C17 C16 C15 . 120.2(4) ?
C17 C16 H16A . 119.9 ?
C15 C16 H16A . 119.9 ?
C16 C17 C18 . 116.4(4) ?
C16 C17 H17A . 121.8 ?
C18 C17 H17A . 121.8 ?
N5 C18 C17 . 116.1(4) ?
N5 C18 C13 . 120.9(3) ?
C17 C18 C13 . 123.0(3) ?
N5 C19 C20 . 115.0(3) ?
N5 C19 C12 . 126.7(3) ?
C20 C19 C12 . 118.3(3) ?
C24 C20 C19 . 116.0(3) ?
C24 C20 C21 . 121.6(3) ?
C19 C20 C21 . 122.5(3) ?
C22 C21 C20 . 118.9(3) ?
C22 C21 H21A . 120.5 ?
C20 C21 H21A . 120.5 ?
C21 C22 C23 . 115.8(3) ?
C21 C22 H22A . 122.1 ?
C23 C22 H22A . 122.1 ?
N3 C23 C22 . 127.2(3) ?
N3 C23 H23A . 116.4 ?
C22 C23 H23A . 116.4 ?
N3 C24 C20 . 119.8(3) ?
N3 C24 C25 . 115.5(3) ?
C20 C24 C25 . 124.7(3) ?
C11 C25 N2 . 121.1(3) ?
C11 C25 C24 . 118.9(3) ?
N2 C25 C24 . 120.0(2) ?
C6 N1 C2 . 123.1(3) ?
C6 N1 Ni1 . 113.6(2) ?
C2 N1 Ni1 . 122.7(2) ?
C25 N2 C8 . 122.1(3) ?
C25 N2 Ni1 . 109.6(2) ?
C8 N2 Ni1 . 127.5(2) ?
C24 N3 C23 . 116.8(3) ?
C24 N3 Ni1 . 108.9(2) ?
C23 N3 Ni1 . 133.3(2) ?
C12 N4 C13 . 115.0(3) ?
C18 N5 C19 . 113.4(3) ?
C1 O1 Ni1 4_565 139.9(2) ?
C1 O2 Ni1 . 119.3(2) ?
C7 O4 Ni1 . 109.4(2) ?
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
Ni1 N1 . 1.921(3) yes
Ni1 N2 . 2.015(3) yes
Ni1 O4 . 2.021(2) yes
Ni1 O2 . 2.155(2) yes
Ni1 N3 . 2.175(3) yes
Ni1 O1 4_566 2.233(2) yes
C1 O2 . 1.231(4) ?
C1 O1 . 1.261(4) ?
C1 C2 . 1.426(4) ?
C2 C3 . 1.322(5) ?
C2 N1 . 1.332(4) ?
C3 C4 . 1.315(5) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.381(5) ?
C4 H4A . 0.9300 ?
C5 C6 . 1.327(5) ?
C5 H5A . 0.9300 ?
C6 N1 . 1.260(4) ?
C6 C7 . 1.527(5) ?
C7 O3 . 1.179(4) ?
C7 O4 . 1.232(4) ?
C8 C9 . 1.374(5) ?
C8 N2 . 1.405(4) ?
C8 H8A . 0.9300 ?
C9 C10 . 1.398(5) ?
C9 H9A . 0.9300 ?
C10 C11 . 1.501(5) ?
C10 H10A . 0.9300 ?
C11 C25 . 1.379(3) ?
C11 C12 . 1.432(4) ?
C12 N4 . 1.323(4) ?
C12 C19 . 1.532(5) ?
C13 N4 . 1.388(5) ?
C13 C14 . 1.395(5) ?
C13 C18 . 1.504(6) ?
C14 C15 . 1.397(6) ?
C14 H14A . 0.9300 ?
C15 C16 . 1.472(7) ?
C15 H15A . 0.9300 ?
C16 C17 . 1.352(6) ?
C16 H16A . 0.9300 ?
C17 C18 . 1.455(5) ?
C17 H17A . 0.9300 ?
C18 N5 . 1.334(5) ?
C19 N5 . 1.367(4) ?
C19 C20 . 1.441(5) ?
C20 C24 . 1.432(5) ?
C20 C21 . 1.471(5) ?
C21 C22 . 1.343(5) ?
C21 H21A . 0.9300 ?
C22 C23 . 1.432(5) ?
C22 H22A . 0.9300 ?
C23 N3 . 1.403(4) ?
C23 H23A . 0.9300 ?
C24 N3 . 1.333(4) ?
C24 C25 . 1.537(4) ?
C25 N2 . 1.380(4) ?
O1 Ni1 4_565 2.233(2) ?
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
_geom_hbond_publ_flag
C4 H4A O2 4_465 0.9300 2.4800 3.190(4) 134.00 yes
C22 H22A O4 1_554 0.9300 2.5600 3.456(4) 162.00 yes
