#------------------------------------------------------------------------------
#$Date: 2016-11-08 22:14:22 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188272 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/40/1544071.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_1544071
loop_
_publ_author_name
'Gural'skiy, Il'ya A.'
'Shylin, Sergii I.'
'Golub, Bohdan O.'
'Ksenofontov, Vadim'
'Fritsky, Igor O.'
'Tremel, Wolfgang'
_publ_section_title
;
 High temperature spin crossover in [Fe(pyrazine){Ag(CN)2}2] and its
 solvate
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              9012
_journal_paper_doi               10.1039/C6NJ01472K
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         '0.5(C16 H8 Ag4 Fe2 N12), 0.5(C4 H6 N2)'
_chemical_formula_sum            'C10 H7 Ag2 Fe N7'
_chemical_formula_weight         496.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-24 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.622(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.734(4)
_cell_length_b                   12.536(6)
_cell_length_c                   9.120(5)
_cell_measurement_reflns_used    759
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.122
_cell_measurement_theta_min      2.545
_cell_volume                     675.8(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            995
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.357
_diffrn_reflns_theta_min         2.544
_exptl_absorpt_coefficient_mu    3.927
_exptl_absorpt_correction_T_max  0.745617
_exptl_absorpt_correction_T_min  0.421829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0743 before and 0.0409 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1031 before and 0.0569 after correction.
 The Ratio of minimum to maximum transmission is 0.56.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 3192 reflections, Rint = 0.0636
 (1970 with I > 3sig(I), Rint = 0.0551)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.442
_exptl_crystal_description       needle
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.200
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.04(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         995
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0389
_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)+(0.0344P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0791
_reflns_Friedel_coverage         0.984
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                889
_reflns_number_total             995
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6nj01472k2.cif
_cod_data_source_block           ig_892_0m
_cod_depositor_comments          'Adding full bibliography for 1544071.cif.'
_cod_original_cell_volume        675.7(6)
_cod_database_code               1544071
_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_max   0.962
_shelx_estimated_absorpt_t_min   0.695
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.48(10) 0.1(1) 0.422(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C4) = Uanis(N4) = Uanis(N3) = Uanis(C3)
Uanis(N1) = Uanis(N2)
Uanis(C1) = Uanis(C2)
4. Others
 Fixed Sof: H6A(0.5) H6B(0.5) H6C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3)
5.b Idealised Me refined with riding coordinates:
 C6(H6A,H6B,H6C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'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
Fe1 Fe -0.6193(4) 0.0000 -0.9180(3) 0.0073(5) Uani 1 2 d S T P . .
Ag1 Ag -0.3537(3) 0.23302(6) -0.3985(2) 0.0222(2) Uani 1 1 d . . . . .
C1 C -0.450(2) 0.1601(9) -0.6237(15) 0.0125(15) Uani 1 1 d . . . . .
N1 N -0.5117(16) 0.1070(8) -0.7414(13) 0.0106(12) Uani 1 1 d . . . . .
C2 C -0.275(2) 0.3265(9) -0.1909(15) 0.0125(15) Uani 1 1 d . . . . .
N2 N -0.2268(16) 0.3891(7) -0.0902(13) 0.0106(12) Uani 1 1 d . . . . .
N4 N -0.915(2) 0.0000 -0.9213(17) 0.0077(10) Uani 1 2 d S T P . .
C4 C -1.0186(17) 0.0914(8) -0.9229(13) 0.0077(10) Uani 1 1 d . . . . .
H4 H -0.9509 0.1575 -0.9249 0.009 Uiso 1 1 calc R . . . .
N5 N -0.402(5) 0.0000 -0.291(3) 0.056(6) Uani 1 2 d S T P . .
N3 N -0.322(2) 0.0000 -0.9141(17) 0.0077(10) Uani 1 2 d S T P . .
C3 C -0.2261(17) 0.0908(8) -0.9216(14) 0.0077(10) Uani 1 1 d . . . . .
H3 H -0.2991 0.1565 -0.9262 0.009 Uiso 1 1 calc R . . . .
C6 C -0.832(4) 0.0000 -0.502(3) 0.036(6) Uani 1 2 d S T P . .
H6A H -0.8780 -0.0716 -0.5494 0.055 Uiso 0.5 1 calc R . . A -1
H6B H -0.8615 0.0510 -0.5916 0.055 Uiso 0.5 1 calc R . . A -1
H6C H -0.9187 0.0206 -0.4454 0.055 Uiso 0.5 1 calc R . . A -1
C5 C -0.590(4) 0.0000 -0.381(3) 0.033(5) Uani 1 2 d S T P . .
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'
Ag Ag -0.8971 1.1015 '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_
_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
N1 Fe1 N1 87.0(6) . 2
N1 Fe1 N2 91.3(3) 2 3_444
N1 Fe1 N2 91.3(3) . 4_454
N1 Fe1 N2 178.2(5) . 3_444
N1 Fe1 N2 178.2(5) 2 4_454
N1 Fe1 N4 89.2(4) 2 .
N1 Fe1 N4 89.2(4) . .
N1 Fe1 N3 90.7(4) 2 .
N1 Fe1 N3 90.7(4) . .
N2 Fe1 N2 90.5(6) 3_444 4_454
N2 Fe1 N4 90.3(4) 3_444 .
N2 Fe1 N4 90.3(4) 4_454 .
N2 Fe1 N3 89.8(4) 3_444 .
N2 Fe1 N3 89.8(4) 4_454 .
N4 Fe1 N3 179.9(7) . .
C1 Ag1 C2 171.7(6) . .
N1 C1 Ag1 170.4(11) . .
C1 N1 Fe1 171.1(10) . .
N2 C2 Ag1 169.9(10) . .
C2 N2 Fe1 174.9(9) . 3_556
C4 N4 Fe1 121.2(6) 2 .
C4 N4 Fe1 121.2(6) . .
C4 N4 C4 117.6(12) . 2
N4 C4 H4 119.6 . .
N4 C4 C3 120.9(9) . 1_455
C3 C4 H4 119.6 1_455 .
C3 N3 Fe1 120.8(6) 2 .
C3 N3 Fe1 120.8(6) . .
C3 N3 C3 118.1(12) . 2
C4 C3 H3 119.4 1_655 .
N3 C3 C4 121.2(9) . 1_655
N3 C3 H3 119.4 . .
H6A C6 H6B 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
N5 C5 C6 179(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.950(11) .
Fe1 N1 1.950(11) 2
Fe1 N2 1.958(11) 4_454
Fe1 N2 1.958(11) 3_444
Fe1 N4 1.974(12) .
Fe1 N3 1.984(12) .
Ag1 C1 2.049(12) .
Ag1 C2 2.069(12) .
C1 N1 1.157(14) .
C2 N2 1.130(14) .
N2 Fe1 1.958(11) 3_556
N4 C4 1.339(12) 2
N4 C4 1.339(12) .
C4 H4 0.9500 .
C4 C3 1.403(9) 1_455
N5 C5 1.13(3) .
N3 C3 1.327(11) .
N3 C3 1.327(11) 2
C3 C4 1.403(9) 1_655
C3 H3 0.9500 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C6 C5 1.47(3) .
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_4
Fe1 N4 C4 C3 -178.6(8) . 1_455
Fe1 N3 C3 C4 -178.5(8) . 1_655
C4 N4 C4 C3 2(2) 2 1_455
C3 N3 C3 C4 -5(2) 2 1_655
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.48(10)
2 0.1(1)
3 0.422(3)
