#------------------------------------------------------------------------------
#$Date: 2022-03-16 01:00:07 +0100 (Wed 16 de Mar de 2022) $
#$Revision: 273710 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/97/7709761.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_7709761
loop_
_publ_author_name
'Setifi, Zouaoui'
'Setifi, Fatima'
'Benmansour Souilamas, Samia'
'Liu, Xiangyu'
'Mague, Joel T.'
'Gomez Garcia, Carlos J.'
'Konieczny, Piotr'
'Reedijk, Jan'
_publ_section_title
;
 A rare example of a double metamagnetic transition leading to 2D and 3D
 long-range order in the two-dimensional pyrazine- and azido-bridged
 cobalt(II) compound [Co(pyz)(N3)2]
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00294A
_journal_year                    2022
_chemical_formula_moiety         'C4 H4 Co N8'
_chemical_formula_sum            'C4 H4 Co N8'
_chemical_formula_weight         223.08
_chemical_name_systematic
;
catena-[bis(μ-azido)(μ-pyrazine)cobalt (II)]ₙ
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2022-01-04 deposited with the CCDC.	2022-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1297(7)
_cell_length_b                   7.1034(3)
_cell_length_c                   6.6093(2)
_cell_measurement_reflns_used    2014
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.552
_cell_measurement_theta_min      5.849
_cell_volume                     710.32(5)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT  (Bruker, 2016)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2016)'
_computing_structure_refinement
'SHELXL-2018/1 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2600
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        72.500
_diffrn_reflns_theta_max         72.530
_diffrn_reflns_theta_min         5.849
_diffrn_source                   'INCOATEC I\mS micro--focus source'
_exptl_absorpt_coefficient_mu    18.666
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.23
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.426
_exptl_transmission_factor_min   0.137
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0636P)²+0.4126P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                360
_reflns_number_total             398
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00294a2.cif
_cod_data_source_block           jtm965a_Cmcm_a
_cod_database_code               7709761
_shelx_shelxl_version_number     2018/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.194
_shelx_estimated_absorpt_t_max   0.707
_shelx_res_file
;
TITL jtm965a_Cmcm_a.res in Cmcm
    jtm965a_Cmcm_a.res
    created by SHELXL-2018/1 at 14:15:49 on 10-Sep-2018
REM Old TITL jtm965a_Cmcm in Cmcm
REM SHELXT solution in Cmcm
REM R1 0.088,  Rweak 0.002,  Alpha 0.074,  Orientation as input
REM Formula found by SHELXT:  C6 Co N6
CELL  1.54178  15.1297   7.1034   6.6093   90.000   90.000   90.000
ZERR    4.000   0.0007   0.0003   0.0002    0.000    0.000    0.000
LATT  7
SYMM -X, -Y, 1/2+Z
SYMM -X, Y, 1/2-Z
SYMM X, -Y, -Z
SFAC C H CO N
UNIT 16 16 4 32
TEMP -123
SIZE 0.02 0.082 0.131
L.S. 5
BOND $H
CONF
ACTA 145
LIST 4
FMAP 2
PLAN 5
WGHT    0.063600    0.412600
FVAR       0.52653
CO1   3    0.500000    0.500000    0.500000    10.25000    0.01173    0.01200 =
         0.01734   -0.00031    0.00000    0.00000
N1    4    0.500000    0.196601    0.500742    10.50000    0.01762    0.01524 =
         0.01545    0.00146    0.00000    0.00000
N2    4    0.409085    0.490897    0.750000    10.50000    0.01427    0.01922 =
         0.02006    0.00000    0.00000    0.00124
N3    4    0.333289    0.542052    0.750000    10.50000    0.01933    0.02406 =
         0.01964    0.00000    0.00000   -0.00056
N4    4    0.260557    0.591410    0.750000    10.50000    0.01675    0.05452 =
         0.04144    0.00000    0.00000    0.00850
C1    1    0.575348    0.097325    0.500637    11.00000    0.01516    0.01800 =
         0.02290    0.00110   -0.00013   -0.00073
AFIX  43
H1    2    0.630196    0.162425    0.501462    11.00000   -1.20000
AFIX   0
HKLF 4




REM  jtm965a_Cmcm_a.res in Cmcm
REM R1 =  0.0353 for     360 Fo > 4sig(Fo)  and  0.0385 for all     398 data
REM     38 parameters refined using      0 restraints

END

WGHT      0.0635      0.4117

REM Highest difference peak  0.471,  deepest hole -0.559,  1-sigma level  0.106
Q1    1   0.5000  0.3211  0.5558  10.50000  0.05    0.47
Q2    1   0.5000  0.6242  0.6444  10.50000  0.05    0.29
Q3    1   0.4288  0.4280  0.8464  11.00000  0.05    0.21
Q4    1   0.4184  0.3012  0.7500  10.50000  0.05    0.20
Q5    1   0.4450  0.2179  0.3263  11.00000  0.05    0.19
;
_shelx_res_checksum              90173
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.500000 0.500000 0.500000 0.0137(3) Uani 1 4 d S T P . .
N1 N 0.500000 0.1966(5) 0.5007(3) 0.0161(7) Uani 1 2 d S T P . .
N2 N 0.4091(2) 0.4909(3) 0.750000 0.0178(7) Uani 1 2 d S T P . .
N3 N 0.33329(18) 0.5421(4) 0.750000 0.0210(6) Uani 1 2 d S T P . .
N4 N 0.26056(18) 0.5914(5) 0.750000 0.0376(8) Uani 1 2 d S T P . .
C1 C 0.57535(18) 0.0973(4) 0.5006(3) 0.0187(6) Uani 1 1 d . . . . .
H1 H 0.630196 0.162425 0.501462 0.022 Uiso 1 1 calc R U . . .
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 0.0117(5) 0.0120(4) 0.0173(5) -0.0003(2) 0.000 0.000
N1 0.0176(16) 0.0152(14) 0.0154(16) 0.0015(7) 0.000 0.000
N2 0.0143(15) 0.0192(15) 0.0201(17) 0.000 0.000 0.0012(7)
N3 0.0193(14) 0.0241(11) 0.0196(14) 0.000 0.000 -0.0006(12)
N4 0.0167(13) 0.055(2) 0.0414(18) 0.000 0.000 0.0085(12)
C1 0.0152(13) 0.0180(15) 0.0229(14) 0.0011(6) -0.0001(6) -0.0007(11)
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 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'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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
N2 Co1 N2 180.0 11_565 3_656 ?
N2 Co1 N2 79.51(13) 11_565 9_666 ?
N2 Co1 N2 100.49(13) 3_656 9_666 ?
N2 Co1 N2 100.49(13) 11_565 . ?
N2 Co1 N2 79.51(13) 3_656 . ?
N2 Co1 N2 180.0 9_666 . ?
N2 Co1 N1 88.18(6) 11_565 9_666 ?
N2 Co1 N1 91.82(6) 3_656 9_666 ?
N2 Co1 N1 88.18(6) 9_666 9_666 ?
N2 Co1 N1 91.82(6) . 9_666 ?
N2 Co1 N1 91.82(6) 11_565 . ?
N2 Co1 N1 88.18(6) 3_656 . ?
N2 Co1 N1 91.82(6) 9_666 . ?
N2 Co1 N1 88.18(6) . . ?
N1 Co1 N1 180.0 9_666 . ?
C1 N1 C1 116.5(3) 12_655 . ?
C1 N1 Co1 121.74(17) 12_655 . ?
C1 N1 Co1 121.74(17) . . ?
N3 N2 Co1 126.91(8) . 2_665 ?
N3 N2 Co1 126.91(8) . . ?
Co1 N2 Co1 100.38(13) 2_665 . ?
N4 N3 N2 179.9(3) . . ?
N1 C1 C1 121.74(17) . 4_556 ?
N1 C1 H1 119.1 . . ?
C1 C1 H1 119.1 4_556 . ?
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 N2 2.151(2) 11_565 ?
Co1 N2 2.151(2) 3_656 ?
Co1 N2 2.151(2) 9_666 ?
Co1 N2 2.151(2) . ?
Co1 N1 2.155(3) 9_666 ?
Co1 N1 2.155(3) . ?
N1 C1 1.340(3) 12_655 ?
N1 C1 1.340(3) . ?
N2 N3 1.203(4) . ?
N3 N4 1.155(4) . ?
C1 C1 1.383(6) 4_556 ?
C1 H1 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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 C1 C1 0.3(4) 12_655 . . 4_556 ?
Co1 N1 C1 C1 -179.44(16) . . . 4_556 ?
