Single-Crystal-to-Single-Crystal Transformation from delta-(BEDT-TTF)4[OsNOCl5]1.33(C6H5NO2)0.67 to beta''"-(BEDT-TTF)3[OsNOCl5]
Zorina, Leokadiya; Simonov, Sergey; Canadell, Enric; Shibaeva, Rimma; Crystals 2 (2012) 627–642; doi:10.3390/cryst2020627

data_1508457
_publ_section_title
;
 Single-Crystal-to-Single-Crystal Transformation from
 delta-(BEDT-TTF)4[OsNOCl5]1.33(C6H5NO2)0.67 to
 beta''"-(BEDT-TTF)3[OsNOCl5]
;
_journal_issue                   2
_journal_name_full               Crystals
_journal_page_first              627
_journal_page_last               642
_journal_paper_doi               10.3390/cryst2020627
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety         '3(C10 H8 S8), Cl5 N O Os'
_chemical_formula_sum            'C30 H24 Cl5 N O Os S24'
_chemical_formula_weight         1551.39
_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
_cell_angle_alpha                91.151(9)
_cell_angle_beta                 93.636(7)
_cell_angle_gamma                102.434(9)
_cell_formula_units_Z            1
_cell_length_a                   7.6672(8)
_cell_length_b                   9.8657(11)
_cell_length_c                   17.9733(12)
_cell_measurement_reflns_used    33846
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.9937
_cell_measurement_theta_min      2.1151
_cell_volume                     1324.2(2)
_computing_cell_refinement
'Collect data collection software, Nonius B.V., 1999'
_computing_data_collection
;
Collect data collection software, Nonius B.V., 1999
;
_computing_data_reduction
;
EVALCCD data reduction software,
An intensity evaluation method: EVAL-14. Albert J. M. Duisenberg, 
Loes M.J. Kroon-Batenburg and Antoine M.M. Schreurs, 
J.Appl.Cryst 36 (2003) p.220-229'
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'Bruker Kappa CCD detector'
_diffrn_measurement_method       'combined \w- and \f-scans'
_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  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26451
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         3.89
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.638
_exptl_absorpt_correction_T_max  0.6693
_exptl_absorpt_correction_T_min  0.4290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
based on intensities of measured equivalent reflections,
SADABS (Sheldrick, 1996)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tooth-like
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.801
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0768P)^2^+2.5829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                4608
_reflns_number_total             5653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file
C30H24Cl5NOOsS24_P-1_crystals-16617_crystals-02-00627-s001_DC192.cif
_cod_data_source_block           i220_5_chateigner
_cod_database_code               1508457