Synthesis and Characterization of Rhenium(III) Complexes with (Ph2PCH2CH2)2NR Diphosphinoamine Ligands
Salvarese, Nicola; Refosco, Fiorenzo; Seraglia, Roberta; Roverso, Marco; Dolmella, Alessandro; Bolzati, Cristina; Dalton Trans.  (2017) –; doi:10.1039/C7DT01032J

data_7043294
_publ_section_title
;
 Synthesis and Characterization of Rhenium(III) Complexes with
 (Ph2PCH2CH2)2NR Diphosphinoamine Ligands
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01032J
_journal_year                    2017
_chemical_formula_moiety         'C29 H31 Br3 N P2 Re'
_chemical_formula_sum            'C29 H31 Br3 N P2 Re'
_chemical_formula_weight         881.42
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-05-29 deposited with the CCDC.
2017-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.3668(5)
_cell_length_b                   17.2508(5)
_cell_length_c                   19.9883(6)
_cell_measurement_reflns_used    14761
_cell_measurement_temperature    298.0(1)
_cell_measurement_theta_max      30.5040
_cell_measurement_theta_min      2.6130
_cell_volume                     5988.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.0(1)
_diffrn_detector_area_resol_mean 16.1274
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details
;
  1 omega   -6.00   88.00   0.2500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1412   77.0000 -120.0000 376

  2 omega   48.00   78.00   0.2500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1412   77.0000    0.0000 120

  3 omega  -47.00   33.00   0.2500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1412  -57.0000  120.0000 320

  4 omega  -48.00   52.00   0.2500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1412  -77.0000 -120.0000 400

  5 omega  -25.00   20.00   0.2500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.2974  -99.0000  120.0000 180

  6 omega  -44.00   47.00   0.2500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.2974   57.0000    0.0000 364

  7 omega  -99.00  -53.00   0.2500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.2974  179.0000  -30.0000 184
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0018935000
_diffrn_orient_matrix_UB_12      0.0019170000
_diffrn_orient_matrix_UB_13      -0.0354202000
_diffrn_orient_matrix_UB_21      0.0407146000
_diffrn_orient_matrix_UB_22      -0.0020979000
_diffrn_orient_matrix_UB_23      -0.0017524000
_diffrn_orient_matrix_UB_31      -0.0022500000
_diffrn_orient_matrix_UB_32      -0.0410274000
_diffrn_orient_matrix_UB_33      -0.0015415000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1284
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61265
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         30.76
_diffrn_reflns_theta_min         2.35
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        0.0(1)
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    8.188
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.496
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         8716
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+12.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                6109
_reflns_number_total             8716
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01032j2.cif
_cod_data_source_block           11
_cod_database_code               7043294