Rigid Bis(tetrathiafulvalenes) Doubly Bridged by Phosphino Groups and Derivatives: Synthesis and Intramolecular Mixed Valence State
Danila, Ion; Biaso, Frédéric; Sidorenkova, Helena; Geoffroy, Michel; Fourmigué, Marc; Levillain, E.; Avarvari, Narcis; Organometallics 28 (2009) 3691–; doi:10.1021/om900107y

data_4069254
_publ_section_title
;
 Rigid Bis(tetrathiafulvalenes) Doubly Bridged by Phosphino Groups and
 Derivatives: Synthesis and Intramolecular Mixed Valence State
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3691
_journal_paper_doi               10.1021/om900107y
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         C52H38O10P2S8W2
_chemical_formula_sum            'C52 H38 O10 P2 S8 W2'
_chemical_formula_weight         1508.94
_chemical_name_common            'trans-(o-DMTTF)2{[W(CO)5]PPh}2, C7H8'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.44(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.098(3)
_cell_length_b                   12.607(3)
_cell_length_c                   15.831(3)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_volume                     2767.1(11)
_computing_cell_refinement       'SELECT, CELL [STOE-IPDS]'
_computing_data_collection       'EXPOSE [STOE-IPDS]'
_computing_data_reduction        'INTEGRATE [STOE-IPDS]'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, Phi. incr. = 1.5'
_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  0.0643
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20810
_diffrn_reflns_theta_full        25.83
_diffrn_reflns_theta_max         25.83
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    4.570
_exptl_absorpt_correction_T_max  0.5870
_exptl_absorpt_correction_T_min  0.4197
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   faceit
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                4119
_reflns_number_total             5298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900107y_si_002.cif
_cod_data_source_block           trans-4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' 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 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2767.1(10)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4069254