High-pressure spin-crossover in a dinuclear Fe(ii) complex.
Shepherd, Helena J.; Rosa, Patrick; Vendier, Laure; Casati, Nicola; Létard, Jean-François; Bousseksou, Azzedine; Guionneau, Philippe; Molnár, Gábor; Physical chemistry chemical physics : PCCP 14 (2012) 5265–5271; doi:10.1039/c2cp23940j

data_7207684
_publ_section_title
;
 High-pressure spin-crossover in a dinuclear Fe(ii) complex.
;
_journal_issue                   15
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              5265
_journal_page_last               5271
_journal_paper_doi               10.1039/c2cp23940j
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C36 H26 Fe2 N16 S4, 2(C H4 O)'
_chemical_formula_sum            'C38 H34 Fe2 N16 O2 S4'
_chemical_formula_weight         984.78
_chemical_name_systematic
;
?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.0(5)
_cell_angle_beta                 112.0(4)
_cell_angle_gamma                89.4(2)
_cell_formula_units_Z            2
_cell_length_a                   14.80(2)
_cell_length_b                   7.69(2)
_cell_length_c                   18.15(11)
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.1440
_cell_measurement_theta_min      2.7486
_cell_volume                     1915(14)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
Absorb Angel (2004) J. Appl. Cryst. 37:486-492
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_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'see _refine_special_details'
_diffrn_ambient_pressure         1600000
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.683
_diffrn_measured_fraction_theta_max 0.695
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3196
_diffrn_reflns_av_sigmaI/netI    0.1983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3749
_diffrn_reflns_theta_full        15.85
_diffrn_reflns_theta_max         15.85
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_correction_T_max  0.397
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Gaussian integration over a grid
of 16 x 16 x 16 points = 4096 total grid points
Based upon method of Burnham (1966)

Data corrected for diamond-anvil cell absorption
Note that exptl_absorpt_correction_tmin and _tmax
the total correction factors applied to the intensities
The individual factors are:
range of dac transmission factors (min-max) 0.497 0.564
range of gasket transmission (min-max) 0.799 0.984
range of P media transmission (min-max) 1.000 1.000

thickness of diamond anvil 1: 1.430 mm, mu = 0.2000 mm-1
thickness of platten 1: 0.000 mm, mu = 0.0000 mm-1

thickness of diamond anvil 2: 1.430 mm, mu = 0.2000 mm-1
thickness of platten 2: 0.000 mm, mu = 0.0000 mm-1

Gasket shadowing corrections were made based upon
Gasket thickness = 220.0 microns, radius = 375.0 microns
Gasket absorption coeff = 27.90 mm-1
REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF
FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.20

Non-absorbing pressure medium
;
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'crystal fills hole of diamond-cell gasket'
_exptl_crystal_F_000             1012
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         625
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1689
_refine_ls_R_factor_gt           0.1180
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1991P)^2^+15.8207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2964
_refine_ls_wR_factor_ref         0.3419
_reflns_number_gt                408
_reflns_number_total             625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cp23940j.txt
_cod_data_source_block           16-kbar
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1915(13)
_cod_original_formula_sum        'C38 H34 Fe2 N16 S4 O2'
_cod_database_code               7207684
_exptl_absorpt_correction_mu     0.000