High temperature spin crossover in [Fe(pyrazine){Ag(CN)2}2] and its solvate
Gural'skiy, Il'ya A.; Shylin, Sergii I.; Golub, Bohdan O.; Ksenofontov, Vadim; Fritsky, Igor O.; Tremel, Wolfgang; New J. Chem. 40 (2016) 9012–; doi:10.1039/C6NJ01472K

data_1544071
_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 \l/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 \l/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/[\s^2^(Fo^2^)+(0.0344P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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'