Rhenium Chemistry of Azooximes: Oxygen Atom Transfer, Azoimine Chelation, and Imine-Oxime Contrast
Indranil Chakraborty; Bikash Kumar Panda; Jaydip Gangopadhyay; Animesh Chakravorty; Inorganic Chemistry 44 (2005) 1054–1060; doi:10.1021/ic0486116

data_4308554
_publ_section_title
;
Rhenium Chemistry of Azooximes: Oxygen Atom Transfer, Azoimine Chelation,
and Imine-Oxime Contrast
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1054
_journal_page_last               1060
_journal_paper_doi               10.1021/ic0486116
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        'laboratory synthesis'
_chemical_formula_sum            'C32 H31 Cl2 N3 O2 P Re'
_chemical_formula_weight         777.67
_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                78.63(3)
_cell_angle_beta                 78.53(3)
_cell_angle_gamma                74.49(3)
_cell_formula_units_Z            2
_cell_length_a                   10.785(2)
_cell_length_b                   10.884(2)
_cell_length_c                   14.212(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     1557.0(6)
_computing_cell_refinement       'Siemens P3/P4-PC V4.27'
_computing_data_collection       'Siemens P3/P4-PC V4.27'
_computing_data_reduction        'Siemens P3/P4-PC V4.27'
_computing_molecular_graphics    'Siemens SHELXTL V5.03 PC'
_computing_publication_material  'Siemens SHELXTL V5.03 PC'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_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  0.0000
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_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5326
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.159
_exptl_absorpt_correction_T_max  0.524
_exptl_absorpt_correction_T_min  0.351
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       parallelopiped
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_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.551
_refine_diff_density_min         -1.655
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_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.079
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_refine_ls_number_reflns         5316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_restrained_S_obs      1.079
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_obs          0.0261
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+1.1002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0726
_refine_ls_wR_factor_obs         0.0666
_reflns_number_observed          5108
_reflns_number_total             5326
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0486116si20041006_031841_3.cif
_cod_data_source_block           5(Y=Me).H2O
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+1.1002P] 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^)+(0.0461P)^2^+1.1002P] 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        1557.0(5)
_cod_database_code               4308554