Co-ligand and Solvent Effects on the Spin-Crossover Behaviors of PtS-type Porous Coordination Polymers.
Chen, Xiang-Yi; Huang, Rong-Bin; Zheng, Lan-Sun; Tao, Jun; Inorganic chemistry 53 (2014) 5246–5252; doi:10.1021/ic500463m

data_4338261
_publ_section_title
;
 Co-ligand and Solvent Effects on the Spin-Crossover Behaviors of PtS-type
 Porous Coordination Polymers.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5246
_journal_page_last               5252
_journal_paper_doi               10.1021/ic500463m
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C55 H40 Fe N6 Se2'
_chemical_formula_sum            'C55 H40 Fe N6 Se2'
_chemical_formula_weight         998.70
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           50
_space_group_name_Hall           '-P 2ab 2b'
_space_group_name_H-M_alt        'P b a n'
_symmetry_space_group_name_Hall  '-P 2ab 2b'
_symmetry_space_group_name_H-M   'P b a n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5637(11)
_cell_length_b                   35.4521(17)
_cell_length_c                   20.8450(17)
_cell_measurement_temperature    220(2)
_cell_volume                     12979.6(15)
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_av_unetI/netI     0.1469
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27972
_diffrn_reflns_theta_full        65.69
_diffrn_reflns_theta_max         65.69
_diffrn_reflns_theta_min         3.54
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.695
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Approximately 66.1% of the unit cell volume comprises a large region of
disordered solvent which could not be modeled as discrete atomic sites.
We employed PLATON SQUEEZE to calculate the contribution to the diffraction
from the solvent region and thereby produced a set of solvent-free diffraction
intensities. SQUEEZE estimated a total count of 724 electrons per unit cell.
According to the final formula which was calculated from TGA combined with 
elemental analysis data, these electrons were assigned to be 20 methanol and 
8 dichloromethane molecules per unit cell. The F(000) value with solvent is 2720,
Mu (mm^-1) value with solvent is 2.531,and crystal density with solvent is 0.680.
;
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         10746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.2018
_refine_ls_R_factor_gt           0.1089
_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^)+(0.0850P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2503
_refine_ls_wR_factor_ref         0.2877
_reflns_number_gt                3255
_reflns_number_total             10746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500463m_si_002.cif
_cod_data_source_block           2S220K
_cod_depositor_comments
'Adding full bibliography for 4338259--4338264.cif.'
_cod_original_cell_volume        12979.5(15)
_cod_database_code               4338261