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_7031545
_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         'C51 H45 Fe N6 P3, 2(Br)'
_chemical_formula_sum            'C51 H45 Br2 Fe N6 P3'
_chemical_formula_weight         1050.5
_chemical_name_systematic
; 
cis-P,N-[Fe(PN^H^-Ph)~3~]Br~2~ (5b)
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   32.0762(14)
_cell_length_b                   35.738(2)
_cell_length_c                   19.252(2)
_cell_measurement_reflns_used    5222
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.3
_cell_volume                     22069(3)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_structure_refinement  'JANA2006 (Petricek, Dusek, Palatinus, 2006)'
_computing_structure_solution    'SUPERFLIP (Petricek, Dusek, Palatinus, 2006)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD'
_diffrn_measurement_method       '\w- and \f-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43656
_diffrn_reflns_theta_full        30
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.845
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.39
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.2643
_exptl_crystal_description       plate
_exptl_crystal_F_000             8544
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
Due to disorder, the solvent molecules in 5b could not be 
resolved and the electron density in the solvent voids 
corresponding to approximately 2.5 MeOH molecules per 
asymmetric unit was removed with procedure SQUEEZE 
of program PLATON.
;
_refine_diff_density_max         0.81
_refine_diff_density_min         -0.50
_refine_ls_abs_structure_details
'  6918 of Friedel pairs used in the refinement'
_refine_ls_abs_structure_Flack   -0.008(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.15
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    169
_refine_ls_number_parameters     581
_refine_ls_number_reflns         15186
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.0159
_refine_ls_shift/su_mean         0.0007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0004I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                11710
_reflns_number_total             15186
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            c4dt00186a2.cif
_cod_data_source_block           5b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' 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 

The following automatic conversions were performed:

data name '_atom_site_site_symmetry_mutiplicity' was replaced with
'_atom_site_site_symmetry_multiplicity' as specified in the
replacement file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        22070(3)
_cod_original_formula_sum        'C51 H45 Br2 Fe1 N6 P3'
_cod_database_code               7031545