Carbon Dioxide Reduction to Silyl-Protected Methanol Catalyzed by an Oxorhenium Pincer PNN Complex
Mazzotta, Michael G.; Xiong, Manxi; Abu-Omar, Mahdi M.; Organometallics  (2017) –; doi:10.1021/acs.organomet.7b00223

data_4087269
_publ_section_title
;
 Carbon Dioxide Reduction to Silyl-Protected Methanol Catalyzed by an
 Oxorhenium Pincer PNN Complex
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.7b00223
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C23 H44 F3 N2 O5 P1 Re1 S1 Si1,C1 F3 O3 S1'
_chemical_formula_sum            'C24 H44 F6 N2 O8 P Re S2 Si'
_chemical_formula_weight         911.99
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2352(4)
_cell_length_b                   13.1124(3)
_cell_length_c                   22.2118(4)
_cell_measurement_reflns_used    20750
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      63.676
_cell_measurement_theta_min      4.944
_cell_volume                     3563.50(16)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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 HKL3000/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  0.071
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20750
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        63.676
_diffrn_reflns_theta_max         63.676
_diffrn_reflns_theta_min         4.944
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    9.198
_exptl_absorpt_correction_T_max  0.252
_exptl_absorpt_correction_T_min  0.068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         3.591
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         5714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0999P)^2^+8.8672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1304
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                5671
_reflns_number_total             5714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00223_si_002.cif
_cod_data_source_block           MM2053
_cod_database_code               4087269
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.226
_shelx_estimated_absorpt_t_max   0.339
_shelx_res_checksum              59372
_shelx_hkl_checksum              59525