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_7043292
_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         'C30 H33 Br3 N P2 Re'
_chemical_formula_sum            'C30 H33 Br3 N P2 Re'
_chemical_formula_weight         895.44
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-04-17
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_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                 111.117(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4502(3)
_cell_length_b                   19.2607(4)
_cell_length_c                   13.4211(3)
_cell_measurement_reflns_used    20498
_cell_measurement_temperature    299.8(4)
_cell_measurement_theta_max      26.4544
_cell_measurement_theta_min      2.0435
_cell_volume                     3002.25(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'SHELXTL NT vers.5.10 (Sheldrick, 1999)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      299.8(4)
_diffrn_detector_area_resol_mean 16.1274
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_details
;
  1 omega   60.00   91.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0165  179.0000   90.0000 124

  2 omega  -57.00   23.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0165  -38.0000  120.0000 320

  3 omega  -56.00   35.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0165  -38.0000    0.0000 364

  4 omega  -48.00   51.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9384   77.0000  -90.0000 396

  5 omega  -18.00   85.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0165   77.0000  150.0000 412

  6 omega   -4.00   88.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0165   38.0000   60.0000 368

  7 omega  -23.00   48.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0165  -77.0000   90.0000 284

  8 omega   -9.00   79.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0165   77.0000  -90.0000 352

  9 omega   10.00   80.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0165 -133.0000  -89.0000 280
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0526762000
_diffrn_orient_matrix_UB_12      -0.0172753000
_diffrn_orient_matrix_UB_13      -0.0276429000
_diffrn_orient_matrix_UB_21      -0.0069590000
_diffrn_orient_matrix_UB_22      0.0200681000
_diffrn_orient_matrix_UB_23      -0.0462177000
_diffrn_orient_matrix_UB_31      0.0301305000
_diffrn_orient_matrix_UB_32      -0.0255813000
_diffrn_orient_matrix_UB_33      -0.0176092000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33079
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.51
_diffrn_reflns_theta_min         2.05
_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    8.168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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    1.981
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+2.0036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0469
_reflns_number_gt                5036
_reflns_number_total             5597
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01032j2.cif
_cod_data_source_block           3
_cod_original_cell_volume        3002.25(12)
_cod_database_code               7043292