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_4082911
_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_absolute_configuration ad
_chemical_formula_moiety         'C21 H35 Br1 Cl1 N2 O2 P1 Re1,Cl6 Sb1'
_chemical_formula_sum            'C21 H35 Br Cl7 N2 O2 P Re Sb'
_chemical_formula_weight         1014.53
_chemical_name_systematic        ' ?'
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 96.053(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.2611(4)
_cell_length_b                   12.5682(7)
_cell_length_c                   15.6445(7)
_cell_measurement_reflns_used    17193
_cell_measurement_temperature    150.00(2)
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     1615.27(14)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
    ORTEP (Johnson, 1976)
    PLATON (Spek, 2003)
;
_computing_publication_material  'SHELX97(Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_structure_solution
;
 Direct methods (SIR2011, Burla et al., in press)
;
_diffrn_ambient_temperature      150.00(2)
_diffrn_measured_fraction_theta_full 0.9540
_diffrn_measured_fraction_theta_max 0.9540
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite 002'
_diffrn_radiation_type           CU-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1040
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17193
_diffrn_reflns_theta_full        67.5
_diffrn_reflns_theta_max         72.34
_diffrn_reflns_theta_min         3.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.287
_exptl_absorpt_correction_T_max  0.5280
_exptl_absorpt_correction_T_min  0.4624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.86
_refine_diff_density_min         -1.44
_refine_ls_abs_structure_details
'Flack H. D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.489(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5469
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.061
_refine_ls_R_factor_gt           0.061
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.1310P)^2^+8.3915P] where P=(Fo^2^+2Fc^2^)/3  '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.167
_refine_ls_wR_factor_ref         0.167
_reflns_Friedel_coverage         0.8897
_reflns_number_gt                5450
_reflns_number_total             5469
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            om500007m_si_002.cif
_cod_data_source_block           RAM318
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
according to
/usr/data/users/saulius/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4082911.cif.
;
_cod_original_formula_sum        'C21 H35 Br1 Cl7 N2 O2 P1 Re1 Sb1'
_cod_database_code               4082911