Spin Crossover in Fe(II)-M(II) Cyanoheterobimetallic Frameworks (M = Ni, Pd, Pt) with 2-Substituted Pyrazines.
Kucheriv, Olesia I.; Shylin, Sergii I.; Ksenofontov, Vadim; Dechert, Sebastian; Haukka, Matti; Fritsky, Igor O.; Gural'skiy, Il'ya A.; Inorganic chemistry 55 (2016) 4906–4914; doi:10.1021/acs.inorgchem.6b00446

data_4347665
_publ_section_title
;
 Spin Crossover in Fe(II)-M(II) Cyanoheterobimetallic Frameworks (M = Ni,
 Pd, Pt) with 2-Substituted Pyrazines.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4906
_journal_page_last               4914
_journal_paper_doi               10.1021/acs.inorgchem.6b00446
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C9 H8 Fe N6 O Pt, 0.35(C5 H6 N2)'
_chemical_formula_sum            'C10.75 H10.1 Fe N6.7 O Pt'
_chemical_formula_weight         500.09
_chemical_name_systematic        Complex
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.23 svn.r3114 for OlexSys, GUI svn.r4973)
;
_cell_angle_alpha                71.954(7)
_cell_angle_beta                 87.867(5)
_cell_angle_gamma                86.289(4)
_cell_formula_units_Z            2
_cell_length_a                   7.6058(3)
_cell_length_b                   9.1866(7)
_cell_length_c                   14.0502(12)
_cell_measurement_reflns_used    1251
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5420
_cell_measurement_theta_min      2.6380
_cell_volume                     931.31(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4957
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.721
_diffrn_reflns_theta_min         2.335
_exptl_absorpt_coefficient_mu    8.286
_exptl_absorpt_correction_T_max  0.4193
_exptl_absorpt_correction_T_min  0.1853
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'Parkin, S., Moezzi, B., Hope, H. (1995). J. Appl. Cryst. 28, 53-56.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       block
_exptl_crystal_F_000             467
_exptl_crystal_size_max          0.1638
_exptl_crystal_size_mid          0.0938
_exptl_crystal_size_min          0.0582
_refine_diff_density_max         13.406
_refine_diff_density_min         -2.787
_refine_diff_density_rms         0.556
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         4957
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0809
_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^)+(0.1602P)^2^+6.3291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2113
_refine_ls_wR_factor_ref         0.2177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4441
_reflns_number_total             4957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00446_si_007.cif
_cod_data_source_block           sh318
_cod_original_cell_volume        931.32(11)
_cod_original_formula_sum        'C10.75 H10.10 Fe N6.70 O Pt'
_cod_database_code               4347665
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.644
_shelx_estimated_absorpt_t_min   0.344
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C9A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C14) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(N8)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
Uanis(C10) = Uanis(C11) = Uanis(N8) = Uanis(C12) = Uanis(C13) = Uanis(N7)
Uanis(C9A) = Uanis(C9B)
3. Others
 Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=1-FVAR(1)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=FVAR(1)
 Fixed Sof: C14(0.35) H14A(0.35) H14B(0.35) H14C(0.35) C13(0.35) H13(0.35)
 N7(0.35) C10(0.35) C11(0.35) H11(0.35) N8(0.35) C12(0.35) H12(0.35)
4.a Rotating group:
 O1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C13(H13), C11(H11), C12(H12)
4.c Fitted hexagon refined as free rotating group:
 C13(N7,C10,C11,N8,C12)
4.d Idealised Me refined as rotating group:
 C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              25156
_shelx_hkl_checksum              32764
_olex2_submission_special_instructions 'No special instructions were received'