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_4317094
_publ_contact_author
;
      Ulrich Abram
      Freie Universitaet  Berlin     
      Institute of Chemistry             
      Fabeckstrasse 34-36                     
      D-14195 Berlin         
      Germany                          
;
_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
;
C38 H36 N2 O2 P2 Re, C37 H34 N2 O2 P2 Re, 2.5(C H2 Cl2), 2(Cl)
;
_chemical_formula_sum            'C77.5 H75 Cl7 N4 O4 P4 Re2'
_chemical_formula_weight         1870.85
_chemical_name_common            '[ReO2(H2L2)2]Cl,[ReO2(H2L1)H2L2]Cl*2.5CH2Cl2'
_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                84.050(10)
_cell_angle_beta                 77.870(10)
_cell_angle_gamma                61.740(10)
_cell_formula_units_Z            2
_cell_length_a                   15.047(2)
_cell_length_b                   15.087(2)
_cell_length_c                   20.609(2)
_cell_measurement_reflns_used    34643
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      2.05
_cell_volume                     4028.8(9)
_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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0724
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34966
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    3.362
_exptl_absorpt_correction_T_max  0.5297
_exptl_absorpt_correction_T_min  0.3436
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   X-Red32
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1858
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.29
_refine_diff_density_max         5.195
_refine_diff_density_min         -2.047
_refine_diff_density_rms         0.338
_refine_ls_extinction_coef       0.0074(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         17415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1312P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1841
_reflns_number_gt                12295
_reflns_number_total             17415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101792j_si_002_4.cif
_cod_data_source_block           jsrehl1pn
_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 
;
_cod_original_formula_sum        'C77.50 H75 Cl7 N4 O4 P4 Re2'
_cod_database_code               4317094