Polymorphism based on molecular stereoisomerism in tris(oxalato) Cr(III) salts of bedt-ttf [bis(ethylenedithio)tetrathiafulvalene]
Martin, Lee; Turner, Scott S.; Day, Peter; Abdul Malik, K. M.; Coles, Simon J.; Hursthouse, Michael B.; Chemical Communications  (1999) 513–; doi:10.1039/a900482c

data_7110454
_publ_section_title
;
 Polymorphism based on molecular stereoisomerism in tris(oxalato) Cr(III)
 salts of bedt-ttf [bis(ethylenedithio)tetrathiafulvalene]
;
_journal_issue                   6
_journal_name_full               'Chemical Communications'
_journal_page_first              513
_journal_paper_doi               10.1039/a900482c
_journal_year                    1999
_chemical_formula_sum            'C53 H39 Cr N O13 S32'
_chemical_formula_weight         1975.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.371(2)
_cell_length_b                   19.518(3)
_cell_length_c                   35.646(2)
_cell_measurement_temperature    150(2)
_cell_volume                     7215.5(18)
_computing_cell_refinement       MADNES
_computing_data_collection       'MADNES (Pflugrath, 1989)'
_computing_data_reduction        ABSURD
_computing_molecular_graphics    'CAMERON (Pearce, Watkin, 1995)'
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'FAST TV Area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.2159
_diffrn_reflns_av_sigmaI/netI    0.3233
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            24400
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_description       block
_exptl_crystal_F_000             4728
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.731
_refine_ls_goodness_of_fit_obs   1.041
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         5599
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.733
_refine_ls_restrained_S_obs      1.042
_refine_ls_R_factor_all          0.1764
_refine_ls_R_factor_obs          0.0655
_refine_ls_shift/esd_max         -0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1243
_refine_ls_wR_factor_obs         0.1033
_reflns_number_observed          2195
_reflns_number_total             5599
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            900482csup1.cif
_cod_data_source_block           s92
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7216(2)
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7110454