Oxygen Atom Transfer from Nitrogenous ReVO Reagents to Diphosphines and Subsequent Transformations. Rhenium(III) Products and Reaction Models
Sibaprasad Bhattacharyya; Indranil Chakraborty; Bimal Kumar Dirghangi; Animesh Chakravorty; Inorganic Chemistry 40 (2001) 286–293; doi:10.1021/ic0005893

data_4319155
_publ_section_title
;
 Oxygen Atom Transfer from Nitrogenous ReVO Reagents to Diphosphines and
 Subsequent Transformations. Rhenium(III) Products and Reaction Models
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              286
_journal_page_last               293
_journal_paper_doi               10.1021/ic0005893
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'laboratory synthesis'
_chemical_formula_sum            'C45 H39 Cl4 N3 O P2 Re'
_chemical_formula_weight         1027.73
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                89.38(3)
_cell_angle_beta                 87.79(3)
_cell_angle_gamma                80.22(3)
_cell_formula_units_Z            2
_cell_length_a                   10.034(2)
_cell_length_b                   10.737(2)
_cell_length_c                   20.357(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     2159.7(8)
_computing_cell_refinement       'Siemens P3/P4 V-4.27'
_computing_data_collection       'Siemens P3/P4 V-4.27'
_computing_data_reduction        'Siemens P3/P4 V-4.27'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0331
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_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6639
_diffrn_reflns_theta_max         23.55
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.173
_exptl_absorpt_correction_T_max  0.248
_exptl_absorpt_correction_T_min  0.180
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Dark
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       Parallelopiped
_exptl_crystal_F_000             1022
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.037
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_refine_ls_number_reflns         6401
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.037
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_obs          0.0303
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+2.2199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0820
_refine_ls_wR_factor_obs         0.0690
_reflns_number_observed          5518
_reflns_number_total             6403
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0005893_1.cif
_cod_data_source_block           656re
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_angle_publ_flag' value 'Y' changed to 'y'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (21
time).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (12 times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+2.2199P] 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^)+(0.0397P)^2^+2.2199P] where P=(Fo^2^+2Fc^2^)/3'.

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

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'heavy atom method' was changed
to 'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2159.7(7)
_cod_database_code               4319155