Further Studies of the Isomeric 1,2,7- and 1,3,6-Re2Cl5(PMe3)3 Compounds
F. Albert Cotton; Evgeny V. Dikarev; Inorganic Chemistry 35 (1996) 4738–4742; doi:10.1021/ic951473n

data_4323863
_publ_section_title
;
 Further Studies of the Isomeric 1,2,7- and 1,3,6-Re2Cl5(PMe3)3 Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4738
_journal_page_last               4742
_journal_paper_doi               10.1021/ic951473n
_journal_volume                  35
_journal_year                    1996
_chemical_compound_source
;
 reaction of Re2Cl4(PMe3)4 with PhICl2 in the presence of PMe3
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'C9 H27 Cl5 P3 Re2'
_chemical_formula_structural     'Re2 Cl5 (P (C H3)3)3'
_chemical_formula_sum            'C9 H27 Cl5 P3 Re2'
_chemical_formula_weight         777.87
_chemical_name_common
;
 Pentachloro-tris(1,3,6-/1,2,7-)-trimethylphosphino-dirhenium (II, III)
;
_chemical_name_systematic
; 
 Pentachloro-tris(1,3,6-/1,2,7-)-trimethylphosphino-dirhenium (II, III)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.77(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.936(5)
_cell_length_b                   8.8206(8)
_cell_length_c                   34.29(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.805
_cell_measurement_theta_min      12.963
_cell_volume                     4517(2)
_computing_cell_refinement       SDP
_computing_data_collection       SDP
_computing_data_reduction        SDP
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1348
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            8255
_diffrn_reflns_theta_max         24.92
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count '300 reflections'
_diffrn_standards_interval_time  '3600 sec.'
_diffrn_standards_number         '3 refl. for orient., 3 refl. for int.'
_exptl_absorpt_coefficient_mu    11.501
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7923
_exptl_absorpt_correction_type   'empirical via \y scans of 6 refl.'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.288
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle-shaped
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.347
_refine_diff_density_min         -4.889
_refine_diff_density_rms         0.316
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_hydrogen_treatment
;
 riding model by HFIX 33 for methyl groups, common U
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         7157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.295
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_obs          0.0448
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0841P)^2^+4.5898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1544
_refine_ls_wR_factor_obs         0.1157
_reflns_number_observed          6377
_reflns_number_total             7926
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic951473n_1.cif
_cod_data_source_block           (1)str1834
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0841P)^2^+4.5898P] 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^)+(0.0841P)^2^+4.5898P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323863