Six-coordinate high-spin iron(ii) complexes with bidentate PN ligands based on 2-aminopyridine - new Fe(ii) spin crossover systems.
Holzhacker, Christian; Calhorda, Maria José; Gil, Adrià; Carvalho, Maria Deus; Ferreira, Liliana P.; Stöger, Berthold; Mereiter, Kurt; Weil, Matthias; Müller, Danny; Weinberger, Peter; Pittenauer, Ernst; Allmaier, Günter; Kirchner, Karl; Dalton transactions (Cambridge, England : 2003) 43 (2014) 11152–11164; doi:10.1039/c4dt00186a

data_7031546
_publ_section_title
;
 Six-coordinate high-spin iron(ii) complexes with bidentate PN ligands
 based on 2-aminopyridine - new Fe(ii) spin crossover systems.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11152
_journal_page_last               11164
_journal_paper_doi               10.1039/c4dt00186a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C38 H36 Fe N6 P2, 2(B F4)'
_chemical_formula_sum            'C38 H36 B2 F8 Fe N6 P2'
_chemical_formula_weight         868.14
_chemical_name_common            '1466 xx4 [Fe(PN-Ph)2(AN)2](BF4)2.solv'
_chemical_name_systematic
; 
[Fe(PN-Ph)2(CH3CN)2](BF4)2.solv
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.129(2)
_cell_angle_beta                 83.943(2)
_cell_angle_gamma                89.942(2)
_cell_formula_units_Z            4
_cell_length_a                   10.7266(13)
_cell_length_b                   20.317(3)
_cell_length_c                   21.130(3)
_cell_measurement_reflns_used    7606
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.08
_cell_measurement_theta_min      2.18
_cell_volume                     4115.0(10)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD'
_diffrn_measurement_method       '\w- and \f-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            67127
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
Platy red crystals from acetonitrile / diethyl ether.
The compound is a disordered solvate with 
an estimated solvent content of about 1/2 acetontrile
molecule per complex. 
Prior to final refinement the disordered solvent 
was removed from the data with procedure SQUEEZE of
program PLATON. The 3 most significant solvent peaks were
C1S     0.2064    0.7788    0.4238
C2S     0.0906    0.7714    0.4698
C3S    -0.0309    0.7624    0.5103
and were thought to represent essentially acetonitrile (one
molecule per two Fe-complexes !!). According to program
PLATON the solvent cavities (2 symmetry equivalent per unit cell)
are located at x,y,z = 0.062, 0.736, 0.486 and -x,-y,-z.
The solvent accessible volume per cavity is 166 A^3 and 332 A^3 
per unit cell.
;
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         23584
_refine_ls_number_restraints     436
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+4.9505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1649
_reflns_number_gt                18402
_reflns_number_total             23584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00186a2.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        4115.1(9)
_cod_original_sg_symbol_Hall     '-P 1  '
_cod_original_sg_symbol_H-M      'P -1  '
_cod_database_code               7031546