#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:31:01 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229884 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/63/7046304.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_7046304
loop_
_publ_author_name
'Rusbridge, Elizabeth K.'
'Peng, Yan'
'Powell, Annie K.'
'Robinson, David'
'Fitzpatrick, Anthony J.'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      1.00  28.00   0.50   11.58    --   16.16  57.00 -60.00   54
  2  ω     -1.00  83.00   0.50   11.58    --   16.16  57.00-150.00  168
  3  ω      9.00  80.00   0.50   11.58    --   16.16  57.00 120.00  142
  4  ω    -27.00  -1.00   0.50   11.58    --  -16.24 -57.00 150.00   52
  5  ω    -81.00 -40.00   0.50   11.58    --  -16.24 -19.00  30.00   82
  6  ω    -65.00   1.00   0.50   11.58    --  -16.24 -63.00 -23.43  132
  7  ω    -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       'ω 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/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/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 > 2σ(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'
_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.
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Fe1 Fe 0.000000 0.500000 0.500000 0.01506(18) Uani 1 2 d S T P
Cl2 Cl 0.21268(9) 0.64576(9) 0.36881(9) 0.02098(19) Uani 1 1 d . . .
Cl3 Cl 0.11848(9) 0.18693(9) 0.41280(9) 0.0214(2) Uani 1 1 d . . .
N4 N 0.2726(3) 0.6734(3) 0.8126(3) 0.0162(4) Uani 1 1 d . . .
N5 N 0.8034(3) 0.6933(4) 1.0606(4) 0.0240(5) Uani 1 1 d . . .
N6 N 0.6043(3) 0.8757(4) 1.2022(3) 0.0215(5) Uani 1 1 d . . .
C7 C 0.4210(4) 0.9161(4) 1.1791(4) 0.0205(5) Uani 1 1 d . . .
H7 H 0.408156 1.012935 1.295253 0.025 Uiso 1 1 calc R . .
C8 C 0.4507(4) 0.6375(4) 0.8363(4) 0.0184(5) Uani 1 1 d . . .
H8 H 0.462861 0.544302 0.718087 0.022 Uiso 1 1 calc R . .
C9 C 0.2574(4) 0.8158(4) 0.9875(4) 0.0200(5) Uani 1 1 d . . .
H9 H 0.131162 0.843124 0.972827 0.024 Uiso 1 1 calc R . .
C10 C 0.6286(4) 0.7360(4) 1.0371(4) 0.0183(5) Uani 1 1 d . . .
H5A H 0.802(6) 0.587(6) 0.928(6) 0.041(9) Uiso 1 1 d . . .
H6 H 0.716(6) 0.930(6) 1.325(6) 0.044(10) Uiso 1 1 d . . .
H5B H 0.921(6) 0.760(5) 1.189(5) 0.036(9) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 -10 3 0.1555
0 -10 7 0.0073
4 9 -8 0.0545
9 -1 -7 0.0082
7 0 4 0.1348
8 -1 3 0.0950
7 -3 4 0.0602
7 -3 4 0.1253
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
Cl2 Fe1 Cl2 180.0 2_566 .
Cl3 Fe1 Cl2 91.63(2) 2_566 2_566
Cl3 Fe1 Cl2 91.63(2) . .
Cl3 Fe1 Cl2 88.37(2) 2_566 .
Cl3 Fe1 Cl2 88.37(2) . 2_566
Cl3 Fe1 Cl3 180.0 . 2_566
N4 Fe1 Cl2 88.54(5) . .
N4 Fe1 Cl2 91.46(5) 2_566 .
N4 Fe1 Cl2 91.46(5) . 2_566
N4 Fe1 Cl2 88.54(5) 2_566 2_566
N4 Fe1 Cl3 90.16(5) . 2_566
N4 Fe1 Cl3 90.16(5) 2_566 .
N4 Fe1 Cl3 89.84(5) 2_566 2_566
N4 Fe1 Cl3 89.84(5) . .
N4 Fe1 N4 180.00(10) 2_566 .
C8 N4 Fe1 120.31(15) . .
C8 N4 C9 118.4(2) . .
C9 N4 Fe1 121.25(16) . .
C10 N5 H5A 114(2) . .
C10 N5 H5B 123(2) . .
H5A N5 H5B 123(3) . .
C7 N6 H6 125(2) . .
C10 N6 C7 121.8(2) . .
C10 N6 H6 114(2) . .
N6 C7 H7 120.2 . .
C9 C7 N6 119.7(2) . .
C9 C7 H7 120.2 . .
N4 C8 H8 118.7 . .
N4 C8 C10 122.6(2) . .
C10 C8 H8 118.7 . .
N4 C9 H9 119.3 . .
C7 C9 N4 121.4(2) . .
C7 C9 H9 119.3 . .
N5 C10 N6 121.6(2) . .
N5 C10 C8 122.2(2) . .
N6 C10 C8 116.1(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 Cl2 2.4900(6) .
Fe1 Cl2 2.4900(6) 2_566
Fe1 Cl3 2.4458(6) 2_566
Fe1 Cl3 2.4458(6) .
Fe1 N4 2.208(2) 2_566
Fe1 N4 2.208(2) .
N4 C8 1.302(3) .
N4 C9 1.377(3) .
N5 C10 1.300(3) .
N5 H5A 1.00(3) .
N5 H5B 0.93(4) .
N6 C7 1.351(3) .
N6 C10 1.351(3) .
N6 H6 0.89(4) .
C7 H7 0.9300 .
C7 C9 1.344(4) .
C8 H8 0.9300 .
C8 C10 1.432(3) .
C9 H9 0.9300 .
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
Fe1 N4 C8 C10 -176.23(18)
Fe1 N4 C9 C7 177.72(19)
N4 C8 C10 N5 177.3(2)
N4 C8 C10 N6 -2.3(4)
N6 C7 C9 N4 -0.7(4)
C7 N6 C10 N5 -178.2(2)
C7 N6 C10 C8 1.5(3)
C8 N4 C9 C7 -0.2(4)
C9 N4 C8 C10 1.7(3)
C10 N6 C7 C9 -0.1(4)
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.3636 -9.7979 3.1478 -0.2934 -0.4791 -0.8273
0.1249 -9.9211 7.4188 -0.4650 -0.7593 -0.4553
3.9374 8.6799 -8.2749 0.6839 0.7210 0.1114
9.2658 -0.5344 -7.4106 0.4080 0.4301 -0.8054
6.6674 0.1910 3.6394 0.8279 -0.5071 -0.2398
7.5001 -0.7437 3.0801 0.7920 -0.4851 -0.3708
7.3192 -3.0243 4.2253 0.6356 -0.6028 -0.4824
7.1280 -2.8069 4.4286 0.6481 -0.6147 -0.4496
