Synthesis and characterisation of oxo- and phenylimido-rhenium(V) complexes containing bidentate phosphinoenolato ligands
Xavier Couillens; Marie Gressier; Reine Turpin; Michèle Dartiguenave; Yvon Coulais; André L. Beauchamp; J. Chem. Soc., Dalton Trans.  (2002) 914–924; doi:10.1039/b106306p

data_7010985
_publ_section_title
;
 Synthesis and characterisation of oxo- and phenylimido-rhenium(V)
 complexes containing bidentate phosphinoenolato ligands
;
_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              914
_journal_page_last               924
_journal_paper_doi               10.1039/b106306p
_journal_year                    2002
_chemical_compound_source        'synthesized by the authors, see text'
_chemical_formula_moiety         'C49 H43 Cl3 N O3 P2 Re'
_chemical_formula_sum            'C49 H43 Cl3 N O3 P2 Re'
_chemical_formula_weight         1048.334
_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           'SHELXL93 (Sheldrick, 1993)'
_cell_angle_alpha                72.09(3)
_cell_angle_beta                 80.05(2)
_cell_angle_gamma                63.03(2)
_cell_formula_units_Z            2
_cell_length_a                   12.027(3)
_cell_length_b                   12.377(3)
_cell_length_c                   17.916(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      20.0
_cell_volume                     2260.0(10)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'NRC-2, NRC-2A (Ahmed et al, 1973)'
_computing_molecular_graphics
'ORTEPII (Johnson (1976) in NRCVAX (Gabe et al (1989))'
_computing_publication_material
'NRCVAX (Gabe et al (1989) and SHELXL93 (Sheldrick (1993))'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       '\w/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus xray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_sigmaI/netI    0.023
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16860
_diffrn_reflns_theta_max         69.80
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        'no decay, variation  1.2'
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    7.86
_exptl_absorpt_correction_T_max  0.416
_exptl_absorpt_correction_T_min  0.078
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'ABSORP in NRCVAX (Gabe et al, 1989)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.5406
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1048.0
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.874
_refine_diff_density_min         -2.180
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       0.00123(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.088
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         8570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+0.2904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1198
_refine_ls_wR_factor_ref         0.1186
_reflns_number_gt                7997
_reflns_number_total             8570
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b106306p.txt
_cod_data_source_block           toul21
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2260.0(9)
_cod_database_code               7010985