Experimental and Theoretical Electron Density Analysis of Copper Pyrazine Nitrate Quasi-Low-Dimensional Quantum Magnets.
Dos Santos, Leonardo H. R.; Lanza, Arianna; Barton, Alyssa M.; Brambleby, Jamie; Blackmore, William J. A.; Goddard, Paul A.; Xiao, Fan; Williams, Robert C.; Lancaster, Tom; Pratt, Francis L.; Blundell, Stephen J.; Singleton, John; Manson, Jamie L.; Macchi, Piero; Journal of the American Chemical Society 138 (2016) 2280–2291; doi:10.1021/jacs.5b12817

data_4130017
_publ_section_title
;
 Experimental and Theoretical Electron Density Analysis of Copper Pyrazine
 Nitrate Quasi-Low-Dimensional Quantum Magnets.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2280
_journal_page_last               2291
_journal_paper_doi               10.1021/jacs.5b12817
_journal_volume                  138
_journal_year                    2016
_chemical_compound_source        'from Jamie L. Manson'
_chemical_formula_moiety         'C4 H4 Cu1 N4 O6'
_chemical_formula_sum            'C4 H4 Cu N4 O6'
_chemical_formula_weight         267.64
_chemical_name_systematic
;
 catena-(bis(\m~2~-pyrazine-N,N')-bis(nitrato-O,O')-copper(ii))
;
_space_group_IT_number           53
_space_group_name_Hall           '-P 2ac 2'
_space_group_name_H-M_alt        'P m n a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      53
_symmetry_space_group_name_Hall  '-P 2ac 2'
_symmetry_space_group_name_H-M   'P m n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             '28-Jul-14 T13:00:26-00:00'
_audit_creation_method           'XD routine XDCIF'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   6.70122(7)
_cell_length_b                   5.11854(5)
_cell_length_c                   11.63508(10)
_cell_measurement_reflns_used    15085
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      57.4610
_cell_measurement_theta_min      3.4930
_cell_measurement_wavelength     0.71073
_cell_volume                     399.089(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Volkov et al, (2006)'
_computing_publication_material  'Volkov et al, (2006)'
_computing_structure_refinement  'Volkov et al, (2006)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9994
_diffrn_measurement_details
;
  1 omega  -38.00   76.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -30.0000 114

  2 omega  -20.00   55.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  150.0000 75

  3 omega  -38.00   76.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -90.0000 114

  4 omega    8.00  122.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       45.5701   57.0000  120.0000 114

  5 omega  -36.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       45.5701  -38.0000 -120.0000 107

  6 omega    2.00  130.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       45.5701   77.0000 -150.0000 128

  7 omega    8.00  122.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       45.5701   57.0000    0.0000 114

  8 omega  -20.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       45.5701  -99.0000  150.0000 121

  9 omega    8.00  122.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       45.5701   57.0000  -60.0000 114

 10 omega  -40.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       45.5701  -79.0000    7.0000 130

 11 omega    2.00  130.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       45.5701   77.0000   30.0000 128

 12 omega   13.00  128.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1401  -63.0000  -30.0000 115

 13 omega    6.00   72.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1401  -25.0000 -180.0000 66

 14 omega    6.00   72.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1401  -25.0000   30.0000 66

 15 omega   36.00  158.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1401   38.0000  -60.0000 122

 16 omega    6.00  134.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1401  -77.0000 -180.0000 128

 17 omega   50.00  158.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1401   50.0000    0.0000 108

 18 omega   11.00  158.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1401   25.0000 -180.0000 147

 19 omega   50.00  158.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1401   50.0000   60.0000 108

 20 omega    2.00  142.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1401  -91.0000    0.0000 140

 21 omega    6.00   72.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1401  -25.0000 -120.0000 66

 22 omega   55.00  158.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1401   63.0000 -150.0000 103

 23 omega   48.00  107.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1401   77.0000  150.0000 59

;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0193232000
_diffrn_orient_matrix_UB_12      0.0407999000
_diffrn_orient_matrix_UB_13      0.0571931000
_diffrn_orient_matrix_UB_21      -0.0527251000
_diffrn_orient_matrix_UB_22      0.1101652000
_diffrn_orient_matrix_UB_23      -0.0211272000
_diffrn_orient_matrix_UB_31      -0.0897020000
_diffrn_orient_matrix_UB_32      -0.0735049000
_diffrn_orient_matrix_UB_33      0.0000770000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24441
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         57.6130
_diffrn_reflns_theta_min         1.7502
_exptl_absorpt_coefficient_mu    2.757
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             266
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.0450(19)
_refine_ls_extinction_expression
;
        Becker, P.J. & Coppens, P. (1974) Acta Cryst., A30, 129-153.
;
_refine_ls_extinction_method     'Becker-Coppens type 1 Lorentzian isotropic'
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2890
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.012
_refine_ls_R_factor_gt           0.009
_refine_ls_shift/su_max          0.0019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
        calc w2 = 1/[s^2^(Fo^2^)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.026
_reflns_number_gt                2695
_reflns_number_total             2933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12817_si_001.cif
_cod_data_source_block           compound1
_cod_original_formula_sum        'C4 H4 Cu1 N4 O6'
_cod_database_code               4130017