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_4317096
_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
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_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         'C38.75 H39 Cl N2 O2.75 P2 Re'
_chemical_formula_sum            'C38.75 H39 Cl N2 O2.75 P2 Re'
_chemical_formula_weight         860.31
_chemical_name_common            '[ReO2(H2L2)2]Cl*3/2MeOH'
_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                93.560(10)
_cell_angle_beta                 95.410(10)
_cell_angle_gamma                109.070(10)
_cell_formula_units_Z            4
_cell_length_a                   11.8360(10)
_cell_length_b                   12.5630(10)
_cell_length_c                   27.119(2)
_cell_measurement_reflns_used    34521
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      29.49
_cell_measurement_theta_min      1.95
_cell_volume                     3775.7(6)
_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      230(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0723
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            40424
_diffrn_reflns_theta_full        29.29
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    3.411
_exptl_absorpt_correction_T_max  0.4922
_exptl_absorpt_correction_T_min  0.3740
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-Red 32'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1718
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.29
_refine_diff_density_max         2.103
_refine_diff_density_min         -1.942
_refine_diff_density_rms         0.370
_refine_ls_extinction_coef       0.0244(6)
_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   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         20155
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1648
_reflns_number_gt                13154
_reflns_number_total             20155
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101792j_si_002_6.cif
_cod_data_source_block           jssw04
_cod_depositor_comments
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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_original_cell_volume        3775.7(5)
_cod_database_code               4317096