Synthesis, Dynamics, and DFT Studies of Rhenium Dicarbonyl PNN Pincer Complexes in Three Different Oxidation States
Pichaandi, Kothanda Rama; Mazzotta, Michael G.; Harwood, John S.; Fanwick, Phillip E.; Abu-Omar, Mahdi M.; Organometallics 33 (2014) 1672–; doi:10.1021/om500007m

data_4082913
_publ_section_title
;
 Synthesis, Dynamics, and DFT Studies of Rhenium Dicarbonyl PNN Pincer
 Complexes in Three Different Oxidation States
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1672
_journal_paper_doi               10.1021/om500007m
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C21 H35 Cl1 N2 O2 P1 Re1,Cl6 Sb1'
_chemical_formula_sum            'C21 H35 Cl7 N2 O2 P Re Sb'
_chemical_formula_weight         934.58
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 102.760(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5329(12)
_cell_length_b                   8.4482(6)
_cell_length_c                   24.9274(18)
_cell_measurement_reflns_used    27490
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      63.686
_cell_measurement_theta_min      2.917
_cell_volume                     3190.3(4)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL2000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27490
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         63.686
_diffrn_reflns_theta_min         2.917
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    20.076
_exptl_absorpt_correction_T_max  0.366
_exptl_absorpt_correction_T_min  0.006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.946
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.136
_refine_diff_density_min         -1.878
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1015P)^2^+21.0450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.1905
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4183
_reflns_number_total             5153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500007m_si_002.cif
_cod_data_source_block           RAM557
_cod_depositor_comments          'Adding full bibliography for 4082913.cif.'
_cod_database_code               4082913
_shelx_estimated_absorpt_t_min   0.108
_shelx_estimated_absorpt_t_max   0.433
_shelxl_version_number           2013-3
_shelx_res_checksum              18861
_shelx_hkl_checksum              55361