Rhenium Complexes with 2-(Diphenylphosphinomethyl)aniline: Formation of a Cyclic, Trinuclear Oxorhenium(V) Core
Jennifer Schroer; Stefan Wagner; Ulrich Abram; Inorganic Chemistry 49 (2010) 10694–10701; doi:10.1021/ic101792j

data_4317092
_publ_contact_author
;
      Ulrich Abram
      Freie Universitaet  Berlin     
      Institute of Chemistry             
      Fabeckstrasse 34-36                     
      D-14195 Berlin         
      Germany                          
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_publ_contact_author_email       abram@chemie.fu-berlin.de
_publ_contact_author_fax         '0049 (0)30 838 52676'
_publ_contact_author_phone       '0049 (0)30 838 54002'
_publ_section_title
;
 Rhenium Complexes with 2-(Diphenylphosphinomethyl)aniline: Formation of a
 Cyclic, Trinuclear Oxorhenium(V) Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10694
_journal_page_last               10701
_journal_paper_doi               10.1021/ic101792j
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C57 H54 Cl3 N3 O6 P3 Re3, O2 C2 H4 Cl4'
_chemical_formula_sum            'C59 H58 Cl7 N3 O8 P3 Re3'
_chemical_formula_weight         1836.74
_chemical_name_common            '[(ReOCl(H2PN))3O3]*4/2CH2Cl2*4/2H2O'
_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-97
_cell_angle_alpha                75.360(10)
_cell_angle_beta                 76.150(10)
_cell_angle_gamma                79.550(10)
_cell_formula_units_Z            2
_cell_length_a                   13.532(2)
_cell_length_b                   16.606(2)
_cell_length_c                   17.555(2)
_cell_measurement_reflns_used    21289
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.16
_cell_measurement_theta_min      2.68
_cell_volume                     3675.0(8)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Wingx
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.1189
_diffrn_reflns_av_sigmaI/netI    0.1691
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38321
_diffrn_reflns_theta_full        29.42
_diffrn_reflns_theta_max         29.42
_diffrn_reflns_theta_min         2.70
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    5.296
_exptl_absorpt_correction_T_max  0.5273
_exptl_absorpt_correction_T_min  0.1587
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   X-Red32
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.196
_refine_diff_density_min         -4.440
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         19692
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.1350
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0806P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1755
_reflns_number_gt                10059
_reflns_number_total             19692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101792j_si_002_2.cif
_cod_data_source_block           jskaese
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
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_cod_database_code               4317092