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_7043295
_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 Cl3 N P2 Re'
_chemical_formula_sum            'C30 H33 Cl3 N P2 Re'
_chemical_formula_weight         762.06
_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             2012-04-16
_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                 112.107(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3950(3)
_cell_length_b                   18.9802(4)
_cell_length_c                   13.2976(4)
_cell_measurement_reflns_used    14169
_cell_measurement_temperature    294.4(1)
_cell_measurement_theta_max      28.8942
_cell_measurement_theta_min      2.0686
_cell_volume                     2898.40(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.47 (release 21-12-2010 CrysAlis171 .NET)
(compiled Dec 21 2010,18:08:13)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.47 (release 21-12-2010 CrysAlis171 .NET)
(compiled Dec 21 2010,18:08:13)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.47 (release 21-12-2010 CrysAlis171 .NET)
(compiled Dec 21 2010,18:08:13)
;
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294.4(1)
_diffrn_detector_area_resol_mean 16.1274
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_details
;
  1 omega  -88.00  -62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1853  179.0000  -90.0000 26

  2 omega  -93.00  -41.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1853  151.0000   13.0000 52

  3 omega   39.00   95.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2634 -151.0000  -30.0000 56

  4 omega  -51.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2634    0.0000  150.0000 127

  5 omega  -78.00   13.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1853  -77.0000  -30.0000 91

  6 omega  -13.00   69.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2634   77.0000  120.0000 82

  7 omega  -11.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2634   77.0000 -120.0000 99

  8 omega  -53.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2634  -38.0000   90.0000 108

  9 omega  -47.00   96.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2634    0.0000  -90.0000 143
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0040226000
_diffrn_orient_matrix_UB_12      -0.0367785000
_diffrn_orient_matrix_UB_13      -0.0101774000
_diffrn_orient_matrix_UB_21      -0.0139693000
_diffrn_orient_matrix_UB_22      -0.0054640000
_diffrn_orient_matrix_UB_23      0.0464520000
_diffrn_orient_matrix_UB_31      -0.0600538000
_diffrn_orient_matrix_UB_32      0.0037358000
_diffrn_orient_matrix_UB_33      -0.0324413000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38682
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         28.96
_diffrn_reflns_theta_min         2.07
_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    4.601
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.47 (release 21-12-2010 CrysAlis171 .NET)
(compiled Dec 21 2010,18:08:13)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.379
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0343P)^2^+0.7678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                5710
_reflns_number_total             6998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01032j2.cif
_cod_data_source_block           2
_cod_original_cell_volume        2898.39(12)
_cod_database_code               7043295