Constructing two 1D coordination polymers and one mononuclear complex by pyrazine- and pyridinedicarboxylic acids under mild and sonochemical conditions: magnetic and CSD studies
Hassanpoor, Azam; Mirzaei, Masoud; Eshtiagh-Hosseini, Hossein; Majcher, Anna; CrystEngComm 20 (2018) 3711–; doi:10.1039/C8CE00573G

data_7230684
_publ_section_title
;
 Constructing two 1D coordination polymers and one mononuclear complex by
 pyrazine- and pyridinedicarboxylic acids under mild and sonochemical
 conditions: magnetic and CSD studies
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              3711
_journal_paper_doi               10.1039/C8CE00573G
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C12 H4 Cu N4 O8, 2(C3 H5 N2 S)'
_chemical_formula_sum            'C18 H14 Cu N8 O8 S2'
_chemical_formula_weight         598.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-11-04
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_audit_update_record
;
2017-05-22 deposited with the CCDC.
2018-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                71.782(4)
_cell_angle_beta                 85.993(4)
_cell_angle_gamma                83.431(4)
_cell_formula_units_Z            1
_cell_length_a                   6.3497(3)
_cell_length_b                   8.0041(4)
_cell_length_c                   11.1477(4)
_cell_measurement_reflns_used    5101
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.0940
_cell_measurement_theta_min      3.7540
_cell_volume                     534.28(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 10.4839
_diffrn_measured_fraction_theta_full 0.9953
_diffrn_measured_fraction_theta_max 0.9953
_diffrn_measurement_details
;
  1 omega  -30.00   55.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.2775   61.0000  -98.0000 85

  2 omega  -86.00   16.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.2775  -61.0000  123.0000 102

  3 omega   36.00   63.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6525 -178.0000  120.0000 27

  4 omega  -16.00   53.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6525  -99.0000   30.0000 69

  5 omega  -92.00  -66.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.2775 -178.0000    0.0000 26

  6 omega  -11.00   23.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.2775  -99.0000 -180.0000 34

  7 omega -101.00  -55.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.2775  178.0000   30.0000 46

  8 omega  -42.00   62.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.2775   57.0000   30.0000 104

  9 omega  -39.00   64.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.2775   38.0000 -120.0000 103

 10 omega  -20.00   30.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.2775  -99.0000    0.0000 50

 11 omega  -94.00   34.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.2775  -19.0000 -120.0000 128

 12 omega   -8.00   26.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6525 -113.0000  -25.7293 34

 13 omega  -66.00  -18.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.2775  119.0000  138.6948 48
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0803028000
_diffrn_orient_matrix_UB_12      0.0023675000
_diffrn_orient_matrix_UB_13      0.0471428000
_diffrn_orient_matrix_UB_21      -0.0102097000
_diffrn_orient_matrix_UB_22      -0.0909388000
_diffrn_orient_matrix_UB_23      0.0109264000
_diffrn_orient_matrix_UB_31      0.0781509000
_diffrn_orient_matrix_UB_32      -0.0226299000
_diffrn_orient_matrix_UB_33      0.0463799000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11423
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.23
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             303
_exptl_crystal_size_max          0.1761
_exptl_crystal_size_mid          0.1342
_exptl_crystal_size_min          0.0819
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2335
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0341
_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/[\s^2^(Fo^2^)+(0.0278P)^2^+0.6199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                2002
_reflns_number_total             2335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00573g2.cif
_cod_data_source_block           ahtd49
_cod_depositor_comments
'Adding full bibliography for 7230684--7230686.cif.'
_cod_database_code               7230684
_chemical_oxdiff_formula         'C9 H8 N4 O4 Cu1 S1 Cl1'
_chemical_oxdiff_usercomment     AHTD49
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N3-H3A
 0.88 with sigma of 0.01
 N4-H4A = N4-H4B
 0.88 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C9(H9)
;