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_4069252
_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         C48.5H34Mo2O10P2S8
_chemical_formula_sum            'C48.5 H34 Mo2 O10 P2 S8'
_chemical_formula_weight         1317.07
_chemical_name_common            'trans-(o-DMTTF)2{[Mo(CO)5]PPh}2, 1.5C7H8'
_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                96.91(1)
_cell_angle_beta                 104.46(1)
_cell_angle_gamma                111.17(1)
_cell_formula_units_Z            2
_cell_length_a                   12.408(2)
_cell_length_b                   13.205(1)
_cell_length_c                   19.364(1)
_cell_measurement_reflns_used    124
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     2786.0(6)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       CCD
_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  0.0653
_diffrn_reflns_av_sigmaI/netI    0.0785
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47770
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.8283
_exptl_absorpt_correction_T_min  0.7970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   wingx
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.049
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         10885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+6.2094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                7817
_reflns_number_total             10885
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900107y_si_002.cif
_cod_data_source_block           trans-3
_cod_depositor_comments
;
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        2786.0
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C48.50 H34 Mo2 O10 P2 S8'
_cod_database_code               4069252