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_4082912
_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'
_chemical_formula_sum            'C21 H35 Cl N2 O2 P Re'
_chemical_formula_weight         600.13
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 107.963(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7184(9)
_cell_length_b                   14.6364(11)
_cell_length_c                   13.3806(6)
_cell_measurement_reflns_used    23024
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      71.929
_cell_measurement_theta_min      4.194
_cell_volume                     2369.4(3)
_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 0.991
_diffrn_measured_fraction_theta_max 0.976
_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  0.068
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23024
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.929
_diffrn_reflns_theta_min         4.194
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    11.849
_exptl_absorpt_correction_T_max  0.623
_exptl_absorpt_correction_T_min  0.202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       needle
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.975
_refine_diff_density_min         -2.073
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4553
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0722P)^2^+6.2734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3707
_reflns_number_total             4553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500007m_si_002.cif
_cod_data_source_block           RAM545
_cod_depositor_comments          'Adding full bibliography for 4082912.cif.'
_cod_database_code               4082912
_shelx_estimated_absorpt_t_min   0.200
_shelx_estimated_absorpt_t_max   0.649
_shelxl_version_number           2013-3
_shelx_res_checksum              57797
_shelx_hkl_checksum              28084