Making Spin-Crossover Crystals by Successive Polymorphic Transformations
Rong-Jia Wei; Bao Li; Jun Tao; Rong-Bin Huang; Lan-Sun Zheng; Zhiping Zheng; Inorganic Chemistry 50 (2011) 1170–1172; doi:10.1021/ic102231j

data_4324484
_publ_contact_author_address
;
Department of Chemistry
Xiamen University
Xiamen 361005
P. R. China
;
_publ_contact_author_email       taojun@xmu.edu.cn
_publ_contact_author_name        'Prof. Jun Tao'
_publ_contact_author_phone       86-592-2188138
_publ_section_title
;
 Making Spin-Crossover Crystals by Successive Polymorphic Transformations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1170
_journal_page_last               1172
_journal_paper_doi               10.1021/ic102231j
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C20 H18 Fe N6 S2'
_chemical_formula_weight         462.37
_chemical_name_systematic
; 
 ? 
;
_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                74.951(5)
_cell_angle_beta                 87.982(5)
_cell_angle_gamma                77.080(5)
_cell_formula_units_Z            4
_cell_length_a                   9.5229(6)
_cell_length_b                   15.4955(8)
_cell_length_c                   16.2637(9)
_cell_measurement_temperature    350(2)
_cell_volume                     2258.3(2)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      350(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Oxford Gemini S Ultra'
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20330
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_T_max  0.9180
_exptl_absorpt_correction_T_min  0.7803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       block-like
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         8788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0472P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                5434
_reflns_number_total             8788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102231j_si_002_1.cif
_cod_data_source_block           IVat350K
_cod_database_code               4324484