An octahedral tetrachlorido Fe(ii) complex with aminopyrazinium ligands from a serendipitous redox synthesis exhibiting magnetic exchange through non-covalent 3-D architectures.
Rusbridge, Elizabeth K.; Peng, Yan; Powell, Annie K.; Robinson, David; Fitzpatrick, Anthony J.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7644–7648; doi:10.1039/c8dt01401a

data_7046304
_publ_section_title
;
 An octahedral tetrachlorido Fe(ii) complex with aminopyrazinium ligands
 from a serendipitous redox synthesis exhibiting magnetic exchange through
 non-covalent 3-D architectures.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7644
_journal_page_last               7648
_journal_paper_doi               10.1039/c8dt01401a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C8 H12 Cl4 Fe N6'
_chemical_formula_sum            'C8 H12 Cl4 Fe N6'
_chemical_formula_weight         389.89
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-10-03 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                115.541(7)
_cell_angle_beta                 110.288(7)
_cell_angle_gamma                96.890(6)
_cell_formula_units_Z            1
_cell_length_a                   7.1768(5)
_cell_length_b                   7.3352(5)
_cell_length_c                   7.8852(6)
_cell_measurement_reflns_used    1466
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      28.4990
_cell_measurement_theta_min      3.7530
_cell_volume                     333.02(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      1.00  28.00   0.50   11.58    --   16.16  57.00 -60.00   54
  2  \w     -1.00  83.00   0.50   11.58    --   16.16  57.00-150.00  168
  3  \w      9.00  80.00   0.50   11.58    --   16.16  57.00 120.00  142
  4  \w    -27.00  -1.00   0.50   11.58    --  -16.24 -57.00 150.00   52
  5  \w    -81.00 -40.00   0.50   11.58    --  -16.24 -19.00  30.00   82
  6  \w    -65.00   1.00   0.50   11.58    --  -16.24 -63.00 -23.43  132
  7  \w    -65.00 -11.00   0.50   11.58    --  -16.24 -57.00 -90.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0922230000
_diffrn_orient_matrix_UB_12      0.0883305000
_diffrn_orient_matrix_UB_13      0.0538884000
_diffrn_orient_matrix_UB_21      -0.0263236000
_diffrn_orient_matrix_UB_22      0.0077711000
_diffrn_orient_matrix_UB_23      -0.0915079000
_diffrn_orient_matrix_UB_31      -0.0561873000
_diffrn_orient_matrix_UB_32      0.0701321000
_diffrn_orient_matrix_UB_33      0.0333660000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2590
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         3.192
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.928
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_description       block
_exptl_crystal_F_000             196
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol/Acetonitrile '
_exptl_crystal_size_max          0.512
_exptl_crystal_size_mid          0.291
_exptl_crystal_size_min          0.137
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.821
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.821
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0321
_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/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1330
_reflns_number_total             1454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01401a2.cif
_cod_data_source_block           af2-1full
_cod_depositor_comments          'Adding full bibliography for 7046304.cif.'
_cod_original_cell_volume        333.02(5)
_cod_database_code               7046304
_chemical_oxdiff_formula         'C8 H12 Cl4 Fe N6'
_chemical_oxdiff_usercomment     'small black crystals'
_reflns_odcompleteness_completeness 98.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9)
;
_shelx_shelxl_version_number     2016/6
_olex2_date_sample_data_collection 2017-03-02
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.265
_oxdiff_exptl_absorpt_empirical_full_min 0.793