p-Tolylimido rhenium(v) complexes - synthesis, X-ray studies, spectroscopic characterization, DFT calculations and catalytic activity.
Machura, Barbara; Gryca, Izabela; Małecki, Jan Grzegorz; Alonso, Francisco; Moglie, Yanina; Dalton transactions (Cambridge, England : 2003) 43 (2014) 2596–2610; doi:10.1039/c3dt52528g

data_7028726
_publ_section_title
;
 p-Tolylimido rhenium(v) complexes - synthesis, X-ray studies,
 spectroscopic characterization, DFT calculations and catalytic activity.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2596
_journal_page_last               2610
_journal_paper_doi               10.1039/c3dt52528g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C31 H26 Cl2 N2 O2 P Re, C2H3N1'
_chemical_formula_sum            'C33 H29 Cl2 N3 O2 P Re'
_chemical_formula_weight         787.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.0403(7)
_cell_length_b                   9.7351(3)
_cell_length_c                   14.5013(5)
_cell_measurement_reflns_used    12301
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2375
_cell_measurement_theta_min      3.4672
_cell_volume                     3111.46(17)
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_molecular_graphics
;XP in SHELXTL/PC (Sheldrick, 1990b)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material
;SHELXL-97 (Sheldrick, 1997) and
 PLATON (Spek, 1990)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20909
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    4.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48531
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlis RED, (2005)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.449
_refine_diff_density_min         -1.347
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0696P)^2^+0.2247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                4576
_reflns_number_total             5134
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52528g.txt
_cod_data_source_block           ren218
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               7028726