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_7043293
_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         'C31 H35 Cl3 N P2 Re'
_chemical_formula_sum            'C31 H35 Cl3 N P2 Re'
_chemical_formula_weight         776.09
_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             2015-07-03
_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                 98.9519(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.44174(12)
_cell_length_b                   14.86579(11)
_cell_length_c                   19.31565(18)
_cell_measurement_reflns_used    25320
_cell_measurement_temperature    297.4
_cell_measurement_theta_max      30.4199
_cell_measurement_theta_min      2.2282
_cell_volume                     3245.39(5)
_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    '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      297.4
_diffrn_detector_area_resol_mean 16.1274
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_details
;
  1 omega  -99.00  -73.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      -25.1216  179.0000   30.0000 52

  2 omega -106.00  -58.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      -25.1216  179.0000 -150.0000 96

  3 omega  -29.00   88.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       25.1216    0.0000 -150.0000 234

  4 omega    2.00   79.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       25.1216   38.0000  -90.0000 154

  5 omega -107.00  -53.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      -25.1216  179.0000   30.0000 108

  6 omega  -32.00   16.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      -25.1216  -93.0000   75.0000 96

  7 omega  -67.00  -40.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      -25.1216   93.0000    6.0000 54

  8 omega  -33.00   47.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      -25.1216   77.0000   90.0000 160

  9 omega   34.00   96.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       25.1216  179.0000  120.0000 124

 10 omega   -5.00   86.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       25.1216   38.0000   90.0000 182

 11 omega   73.00   98.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       25.1216   77.0000 -150.0000 50

 12 omega   -8.00   47.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       25.1216   77.0000 -150.0000 110

 13 omega  -33.00   58.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       25.1216  -77.0000 -150.0000 182

 14 omega   -8.00   98.00   0.5000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       25.1216   77.0000  -30.0000 212
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0531318000
_diffrn_orient_matrix_UB_12      0.0117818000
_diffrn_orient_matrix_UB_13      -0.0221830000
_diffrn_orient_matrix_UB_21      -0.0332162000
_diffrn_orient_matrix_UB_22      -0.0144235000
_diffrn_orient_matrix_UB_23      0.0260615000
_diffrn_orient_matrix_UB_31      0.0033826000
_diffrn_orient_matrix_UB_32      0.0439301000
_diffrn_orient_matrix_UB_33      0.0145129000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            60358
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         30.49
_diffrn_reflns_theta_min         2.23
_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    4.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56755
_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            orange
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.076
_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     339
_refine_ls_number_reflns         9337
_refine_ls_number_restraints     287
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+1.1712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0536
_reflns_number_gt                7949
_reflns_number_total             9337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01032j2.cif
_cod_data_source_block           4
_cod_database_code               7043293