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_7043297
_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         'C28 H29 Cl3 N P2 Re'
_chemical_formula_sum            'C28 H29 Cl3 N P2 Re'
_chemical_formula_weight         734.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
_shelx_SHELXL_version_number      '2016/6'
;
_audit_update_record
;
2017-05-29 deposited with the CCDC.
2017-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.822(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9425(3)
_cell_length_b                   14.9601(3)
_cell_length_c                   25.6721(6)
_cell_measurement_reflns_used    14563
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      29.7210
_cell_measurement_theta_min      2.6180
_cell_volume                     5945.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1274
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_details
;
  1 omega    9.00   81.00   0.5000    7.3050
omega____ theta____ kappa____ phi______ frames
    -       19.8910   57.0000  -30.0000 144

  2 omega  -22.00   93.00   0.5000    7.3050
omega____ theta____ kappa____ phi______ frames
    -       19.8910   19.0000  -90.0000 230

  3 omega  -24.00   18.00   0.5000    7.3050
omega____ theta____ kappa____ phi______ frames
    -      -19.9692  -99.0000   30.0000 84

  4 omega   29.00   77.00   0.5000    7.3050
omega____ theta____ kappa____ phi______ frames
    -       19.8910 -124.0000 -124.6606 96

  5 omega  -49.00   41.00   0.5000    7.3050
omega____ theta____ kappa____ phi______ frames
    -       19.8910  -57.0000  -90.0000 180

  6 omega   -2.00   66.00   0.5000    7.3050
omega____ theta____ kappa____ phi______ frames
    -       19.8910   57.0000 -180.0000 136

  7 omega   34.00   80.00   0.5000    7.3050
omega____ theta____ kappa____ phi______ frames
    -       19.8910  179.0000 -150.0000 92

  8 omega    2.00   89.00   0.5000    7.3050
omega____ theta____ kappa____ phi______ frames
    -       19.8910   57.0000   60.0000 174

  9 omega   16.00   82.00   0.5000    7.3050
omega____ theta____ kappa____ phi______ frames
    -       19.8910 -132.0000   91.0131 132

 10 omega  -23.00   21.00   0.5000    7.3050
omega____ theta____ kappa____ phi______ frames
    -      -19.9692  -99.0000 -150.0000 88

 11 omega  -20.00   45.00   0.5000    7.3050
omega____ theta____ kappa____ phi______ frames
    -      -19.9692   57.0000 -180.0000 130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0238620000
_diffrn_orient_matrix_UB_12      -0.0404152000
_diffrn_orient_matrix_UB_13      0.0021259000
_diffrn_orient_matrix_UB_21      0.0106957000
_diffrn_orient_matrix_UB_22      0.0094921000
_diffrn_orient_matrix_UB_23      -0.0247024000
_diffrn_orient_matrix_UB_31      0.0376225000
_diffrn_orient_matrix_UB_32      0.0228944000
_diffrn_orient_matrix_UB_33      0.0139714000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            46862
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        27.010
_diffrn_reflns_theta_max         29.922
_diffrn_reflns_theta_min         2.286
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.483
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7942
_refine_ls_number_restraints     334
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+1.3850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0537
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6311
_reflns_number_total             7942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01032j2.cif
_cod_data_source_block           10
_cod_database_code               7043297