Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 2. New Reactions Involving Dimethylphenylphosphine
F. Albert Cotton; Evgeny V. Dikarev; Marina A. Petrukhina; Inorganic Chemistry 37 (1998) 1949–1958; doi:10.1021/ic971522r

data_4322750
_publ_section_title
;
 Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 2. New
 Reactions Involving Dimethylphenylphosphine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1949
_journal_page_last               1958
_journal_paper_doi               10.1021/ic971522r
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source
;
 Compound was prepared by stirring a suspension of [Bu4N]2[Re2Cl8]
 in benzene with an excess of PMe2Ph for 4 days at room
 temperature. Single crystals were obtained by slow diffusion of
 isomeric hexanes into dichloromethane solution.
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'Re2 Cl5 (P ((C H3)2 C6 H5))3'
_chemical_formula_structural     1,2,7-Re2Cl5(PMe2Ph)3
_chemical_formula_sum            'C24 H33 Cl5 P3 Re2'
_chemical_formula_weight         964.06
_chemical_melting_point          ?
_chemical_name_common
;
 Pentachloro-tris(dimethylphenylphosphine)-di-rhenium,
 1,2,7-isomer
;
_chemical_name_systematic
; 
 Pentachloro-tris(dimethylphenylphosphine)-di-rhenium
;
_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
_cell_angle_alpha                101.34(2)
_cell_angle_beta                 92.81(2)
_cell_angle_gamma                90.80(2)
_cell_formula_units_Z            2
_cell_length_a                   9.350(3)
_cell_length_b                   11.102(1)
_cell_length_c                   14.558(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.061
_cell_measurement_theta_min      17.053
_cell_volume                     1479.5(6)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 V.5 (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w
_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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6591
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        2.2
_diffrn_standards_interval_count 600
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.803
_exptl_absorpt_correction_T_max  0.9996
_exptl_absorpt_correction_T_min  0.4517
_exptl_absorpt_correction_type   'empirical, via \y scans'
_exptl_crystal_colour            green-brown
_exptl_crystal_density_diffrn    2.164
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.499
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.083
_refine_ls_goodness_of_fit_obs   1.100
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_restrained_S_obs      1.100
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_obs          0.0236
_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^)+(0.0305P)^2^+3.4414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0629
_refine_ls_wR_factor_obs         0.0605
_reflns_number_observed          3683
_reflns_number_total             4081
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971522r_1.cif
_cod_data_source_block           1,2,7-Re2Cl5(PMe2Ph)3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+3.4414P] 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^)+(0.0305P)^2^+3.4414P] 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               4322750