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_7043296
_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_absolute_configuration ad
_chemical_formula_moiety         'C29 H31 Cl3 N P2 Re, C3 H7 N O'
_chemical_formula_sum            'C32 H38 Cl3 N2 O P2 Re'
_chemical_formula_weight         821.13
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-07-03
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_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            4
_cell_length_a                   12.61584(9)
_cell_length_b                   14.38916(10)
_cell_length_c                   18.04782(13)
_cell_measurement_reflns_used    34742
_cell_measurement_temperature    302.3(9)
_cell_measurement_theta_max      32.7214
_cell_measurement_theta_min      2.1426
_cell_volume                     3276.24(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
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_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      302.3(9)
_diffrn_detector_area_resol_mean 16.1274
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
  1 omega  -26.00   95.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       27.2035   13.0000 -179.0000 242

  2 omega   18.00   69.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       27.2035  -99.0000   30.0000 102

  3 omega -103.00  -53.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2035  179.0000 -150.0000 100

  4 omega  -48.00   40.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2035   57.0000  150.0000 176

  5 omega   -3.00   39.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       27.2035   77.0000  120.0000 84

  6 omega  -46.00   69.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       27.2035  -19.0000  -30.0000 230

  7 omega   -3.00   97.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       27.2035   77.0000  -90.0000 200

  8 omega   -2.00   97.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       27.2035   77.0000 -180.0000 198

  9 omega  -24.00   69.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       27.2035  -99.0000 -120.0000 186

 10 omega   -3.00   97.00   0.5000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       27.2035   77.0000    0.0000 200
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0008016000
_diffrn_orient_matrix_UB_12      -0.0143460000
_diffrn_orient_matrix_UB_13      0.0376013000
_diffrn_orient_matrix_UB_21      0.0097561000
_diffrn_orient_matrix_UB_22      -0.0463897000
_diffrn_orient_matrix_UB_23      -0.0113486000
_diffrn_orient_matrix_UB_31      0.0553842000
_diffrn_orient_matrix_UB_32      0.0083726000
_diffrn_orient_matrix_UB_33      0.0014570000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            68698
_diffrn_reflns_theta_full        30.49
_diffrn_reflns_theta_max         32.80
_diffrn_reflns_theta_min         2.15
_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    4.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
'Flack H D (1983), Acta Cryst. A39, 876-881, 4986 Friedel pairs'
;
_refine_ls_abs_structure_Flack   -0.018(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         11414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0181
_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^)+(0.0171P)^2^+0.7487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0380
_refine_ls_wR_factor_ref         0.0392
_reflns_number_gt                10837
_reflns_number_total             11414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01032j2.cif
_cod_data_source_block           1
_cod_database_code               7043296