Rhenium Complex with Noninnocent Dioxolene Ligand: Combined Experimental and ab Initio Study of [(3,5-di-tert-Bu2C6H2O2)ReCl3(OPPh3)].
Abramov, Pavel A.; Gritsan, Nina P.; Suturina, Elizaveta A.; Bogomyakov, Artem S.; Sokolov, Maxim N.; Inorganic chemistry 54 (2015) 6727–6735; doi:10.1021/acs.inorgchem.5b00407

data_4343533
_publ_section_title
;
 Rhenium Complex with Noninnocent Dioxolene Ligand: Combined Experimental
 and ab Initio Study of [(3,5-di-tert-Bu2C6H2O2)ReCl3(OPPh3)].
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6727
_journal_page_last               6735
_journal_paper_doi               10.1021/acs.inorgchem.5b00407
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C32 H35 Cl3 O3 P Re'
_chemical_formula_weight         791.12
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5060(3)
_cell_length_b                   17.3013(7)
_cell_length_c                   19.4327(7)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.35
_cell_volume                     3196.0(2)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2004)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  'CIFTAB-97 (Sheldrick, 1998)'
_computing_structure_refinement  SHELXL-2013
_computing_structure_solution    SHELXS-2013
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_laue_measured_fraction_full 0.980
_diffrn_reflns_laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23260
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.693
_diffrn_reflns_theta_min         2.096
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.134
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_correction_T_min  0.351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       leaf
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.488
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 2443 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.011(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0217P)^2^+9.1489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.751
_reflns_friedel_fraction_full    0.940
_reflns_friedel_fraction_max     0.920
_reflns_number_gt                6151
_reflns_number_total             7076
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5b00407_si_001.cif
_cod_data_source_block           223
_cod_depositor_comments
'Adding full bibliography for 4343533--4343534.cif.'
_cod_database_code               4343533
_shelx_estimated_absorpt_t_min   0.351
_shelx_estimated_absorpt_t_max   0.733
_shelxl_version_number           2013-4
_shelx_res_checksum              22680
_shelx_hkl_checksum              47834