Thermal and pressure-induced spin crossover in a novel three-dimensional Hoffman-like clathrate complex
Shepherd, Helena J.; Bartual-Murgui, Carlos; Molnár, Gábor; Real, José Antonio; Muñoz, M. Carmen; Salmon, Lionel; Bousseksou, Azzedine; New Journal of Chemistry 35 (2011) 1205–; doi:10.1039/c0nj00845a

data_7052643
_publ_section_title
;
 Thermal and pressure-induced spin crossover in a novel
 three-dimensional Hoffman-like clathrate complex
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1205
_journal_paper_doi               10.1039/c0nj00845a
_journal_volume                  35
_journal_year                    2011
_chemical_formula_moiety         '0.25(C56 H32 Ag4 Fe2 N16)'
_chemical_formula_sum            'C14 H8 Ag Fe0.5 N4'
_chemical_formula_weight         368.04
_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_date             2010-11-29
_audit_creation_method
;
Olex2 1.1-beta
(compiled 2010.09.30 svn.r1450, GUI svn.r3284)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.411(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6204(4)
_cell_length_b                   10.8948(5)
_cell_length_c                   13.3105(5)
_cell_measurement_reflns_used    2158
_cell_measurement_temperature    220
_cell_measurement_theta_max      29.0122
_cell_measurement_theta_min      3.5632
_cell_volume                     1388.89(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_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    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      220.0
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_details
;
1 omega -90.00 23.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- -18.3269 0.0000 -30.0000 113

2 omega -90.00 -64.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- -18.3269 179.0000 -90.0000 26

3 omega -40.00 -15.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- -18.3269 -37.0000 -120.0000 25

4 omega -12.00 38.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- 18.5612 84.0000 -128.0000 50
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0127488000
_diffrn_orient_matrix_UB_12      0.0566904000
_diffrn_orient_matrix_UB_13      0.0255021000
_diffrn_orient_matrix_UB_21      -0.0609368000
_diffrn_orient_matrix_UB_22      -0.0084323000
_diffrn_orient_matrix_UB_23      0.0252227000
_diffrn_orient_matrix_UB_31      0.0399843000
_diffrn_orient_matrix_UB_32      -0.0309310000
_diffrn_orient_matrix_UB_33      0.0397813000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5937
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.0122
_diffrn_reflns_theta_min         3.5632
_exptl_absorpt_coefficient_mu    1.944
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.579
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0722P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                1910
_reflns_number_total             3161
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00845a.txt
_cod_data_source_block           Fe(bpac)Ag(CN)2
_cod_original_formula_sum        'C14 H8 Ag Fe0.50 N4'
_cod_database_code               7052643
_chemical_oxdiff_usercomment     220K
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32