#------------------------------------------------------------------------------
#$Date: 2017-04-05 11:32:09 +0200 (Wed 05 de Apr de 2017) $
#$Revision: 195019 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/75/7227517.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_7227517
loop_
_publ_author_name
'Orsi, Angelica'
'Price, David J.'
'Kahr, Jürgen'
'Pillai, Renjith S.'
'Sneddon, Scott'
'Cao, Shuai'
'Benoit, Virginie'
'Łozińska, Magdalena M.'
'Cordes, David B.'
'Slawin, Alexandra M. Z.'
'Llewellyn, Philip L.'
'Casely, Ian'
'Ashbrook, Sharon E.'
'Maurin, Guillaume'
'Wright, Paul A.'
_publ_section_title
;
 Porous zinc and cobalt 2-nitroimidazolate frameworks with six-membered
 ring windows and a layered cobalt 2-nitroimidazolate polymorph
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1377
_journal_paper_doi               10.1039/C6CE02476A
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C6 H4 Co N6 O4'
_chemical_formula_sum            'C6 H4 Co N6 O4'
_chemical_formula_weight         283.07
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d'
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-08-02
_audit_creation_method           'by CrystalStructure 4.2'
_audit_update_record
;
2016-09-27 deposited with the CCDC.
2017-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   6.025(18)
_cell_length_b                   6.025(18)
_cell_length_c                   26.95(8)
_cell_measurement_reflns_used    375
_cell_measurement_temperature    173
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      7.53
_cell_volume                     978(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r2'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r2'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 29.257
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.2823
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            6242
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.645
_diffrn_reflns_theta_max         67.645
_diffrn_reflns_theta_min         6.571
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.988
_exptl_absorpt_correction_T_max  0.657
_exptl_absorpt_correction_T_min  0.091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             564.00
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.43
_refine_ls_extinction_coef       0.0027(16)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     30
_refine_ls_number_reflns         273
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0977
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.1570P)²+2.8079P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2787
_refine_ls_wR_factor_ref         0.2973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                223
_reflns_number_total             273
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c6ce02476a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7227517--7227518.cif.'
_cod_database_code               7227517
_shelx_res_file
;

    shelxl.res created by SHELXL-2014/7

TITL JKPW14
CELL  1.54187 6.02530 6.02530 26.94960 90.00000 90.00000 90.00000
ZERR  4 0.01755 0.01755 0.07913 0.00000 0.00000 0.00000
LATT 2
SYMM    +X, .50-Y,    +Z
SYMM .25+Y, .25+X, .75+Z
SYMM .25+Y, .25-X, .75+Z
SYMM    -X,    +Y,    +Z
SYMM    -X, .50-Y,    +Z
SYMM .75-Y, .25+X, .75+Z
SYMM .75-Y, .25-X, .75+Z
SFAC C H N O CO
UNIT 24 16 24 16 4
L.S. 20
FMAP 2
PLAN 5
WPDB -2
HTAB
BOND $H
CONF
LIST 4
TEMP -100.0
ACTA
SIZE 0.030 0.030 0.030
WGHT    0.157000    2.807900
EXTI    0.002646
FVAR       1.38178
CO1   5    0.000000    0.750000    0.125000    10.12500    0.05991    0.05991 =
         0.12186    0.00000    0.00000    0.00000
O1    4    0.680482    0.750000    0.194154    10.50000    0.11159    0.07602 =
         0.06520    0.00000   -0.02146    0.00000
N1    3    0.500000    0.750000    0.172665    10.25000    0.08765    0.07345 =
         0.05905    0.00000    0.00000    0.00000
N3    3    0.310290    0.750000    0.094572    10.50000    0.08463    0.06565 =
         0.05690    0.00000   -0.00746    0.00000
C2    1    0.500000    0.750000    0.120007    10.25000    0.07748    0.05347 =
         0.06291    0.00000    0.00000    0.00000
C4    1    0.387169    0.750000    0.046553    10.50000    0.06801    0.07637 =
         0.07159    0.00000    0.00163    0.00000
AFIX  43
H4    2    0.296391    0.750000    0.017731    10.50000   -1.20000
AFIX   0
HKLF 4

REM  JKPW14
REM R1 =  0.0977 for     223 Fo > 4sig(Fo)  and  0.1173 for all     273 data
REM     30 parameters refined using      0 restraints

END

WGHT      0.1562      2.7943

REM No hydrogen bonds found for HTAB generation

REM Highest difference peak  0.572,  deepest hole -0.433,  1-sigma level  0.111
Q1    1   0.5000  0.2500  0.1101  10.25000  0.05    0.57
Q2    1   0.1748  0.7500  0.1003  10.50000  0.05    0.39
Q3    1   0.0000  0.7500  0.0095  10.25000  0.05    0.29
Q4    1   0.5000  0.7500  0.0574  10.25000  0.05    0.26
Q5    1   0.3417  0.4083  0.1250  10.50000  0.05    0.26
;
_shelx_res_checksum              12733
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y+1/2, z'
'y+1/4, x+1/4, z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+3/4'
'-y+3/4, -x+1/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'y+3/4, x+3/4, z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+5/4'
'-y+5/4, -x+3/4, z+5/4'
'-x, -y, -z'
'-x, y-1/2, -z'
'-y-1/4, -x-1/4, -z-3/4'
'-y-1/4, x-1/4, -z-3/4'
'x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-3/4'
'y-3/4, x-1/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y, -z+1/2'
'-y+1/4, -x+1/4, -z-1/4'
'-y+1/4, x+1/4, -z-1/4'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z-1/4'
'y-1/4, x+1/4, -z-1/4'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.0000 0.7500 0.1250 0.081(2) Uani 1 8 d S T P
O1 O 0.6805(16) 0.7500 0.1942(3) 0.084(3) Uani 1 2 d S T P
N1 N 0.5000 0.7500 0.1727(5) 0.073(4) Uani 1 4 d S T P
N3 N 0.3103(17) 0.7500 0.0946(3) 0.069(3) Uani 1 2 d S T P
C2 C 0.5000 0.7500 0.1200(6) 0.065(4) Uani 1 4 d S T P
C4 C 0.387(2) 0.7500 0.0466(4) 0.072(3) Uani 1 2 d S T P
H4 H 0.2964 0.7500 0.0177 0.086 Uiso 1 2 calc R U P
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.060(2) 0.060(2) 0.122(4) 0.000 0.000 0.000
O1 0.112(7) 0.076(5) 0.065(5) 0.000 -0.021(5) 0.000
N1 0.088(10) 0.073(8) 0.059(8) 0.000 0.000 0.000
N3 0.085(7) 0.066(5) 0.057(5) 0.000 -0.007(5) 0.000
C2 0.077(11) 0.053(8) 0.063(9) 0.000 0.000 0.000
C4 0.068(7) 0.076(7) 0.072(6) 0.000 0.002(5) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0311 0.0180
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0492 0.0322
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Co Co -2.3653 3.6143
;
International Tables for Crystallography
(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
N3 Co1 N3 132.6(5) . 5
N3 Co1 N3 99.29(19) . 20_666
N3 Co1 N3 99.29(19) 5 20_666
N3 Co1 N3 99.29(19) . 19_666
N3 Co1 N3 99.29(19) 5 19_666
N3 Co1 N3 132.6(5) 20_666 19_666
O1 N1 O1 123.9(13) 5_655 .
O1 N1 C2 118.0(7) 5_655 .
O1 N1 C2 118.0(7) . .
C2 N3 C4 101.3(10) . .
C2 N3 Co1 125.4(7) . .
C4 N3 Co1 133.4(8) . .
N3 C2 N3 118.1(13) . 5_655
N3 C2 N1 120.9(7) . .
N3 C2 N1 121.0(7) 5_655 .
C4 C4 N3 109.7(7) 5_655 .
C4 C4 H4 125.2 5_655 .
N3 C4 H4 125.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N3 2.042(11) .
Co1 N3 2.042(11) 5
Co1 N3 2.042(11) 20_666
Co1 N3 2.042(11) 19_666
O1 N1 1.232(11) .
N1 O1 1.232(11) 5_655
N1 C2 1.42(2) .
N3 C2 1.333(12) .
N3 C4 1.375(15) .
C2 N3 1.333(12) 5_655
C4 C4 1.36(3) 5_655
C4 H4 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C4 N3 C2 N3 0.000(0) . 5_655
Co1 N3 C2 N3 180.000(1) . 5_655
C4 N3 C2 N1 180.000(0) . .
Co1 N3 C2 N1 0.000(1) . .
O1 N1 C2 N3 0.000(1) 5_655 .
O1 N1 C2 N3 180.000(1) . .
O1 N1 C2 N3 180.000(1) 5_655 5_655
O1 N1 C2 N3 0.000(1) . 5_655
C2 N3 C4 C4 0.000(1) . 5_655
Co1 N3 C4 C4 180.000(1) . 5_655
