Oxygen Atom Transfer and Intramolecular Nitrene Transfer in a Rhenium β-Diketiminate Complex.
Lohrey, Trevor D.; Bergman, Robert G.; Arnold, John; Inorganic chemistry 55 (2016) 11993–12000; doi:10.1021/acs.inorgchem.6b02122

data_4349232
_publ_section_title
;
 Oxygen Atom Transfer and Intramolecular Nitrene Transfer in a Rhenium
 \b-Diketiminate Complex.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11993
_journal_page_last               12000
_journal_paper_doi               10.1021/acs.inorgchem.6b02122
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C33 H51 Cl2 N2 O2 Re'
_chemical_formula_weight         764.89
_chemical_name_common            OReCl2(BDI)
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_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                   8.874(4)
_cell_length_b                   18.951(9)
_cell_length_c                   20.467(9)
_cell_measurement_reflns_used    15611
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.27
_cell_measurement_theta_min      2.58
_cell_volume                     3442(3)
_computing_cell_refinement       'SAINT V8.37A Bruker, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker, Madison WI'
_computing_data_reduction        'SAINT V8.37A Bruker, Madison WI'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 Bruker, Madison WI'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'phi and omega shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            61894
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        27.710
_diffrn_reflns_theta_max         40.271
_diffrn_reflns_theta_min         2.583
_diffrn_source                   'Advanced Light Source, station 11.3.1'
_exptl_absorpt_coefficient_mu    4.542
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.5452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 - Bruker AXS, Madison WI'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       lath
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_refine_diff_density_max         3.824
_refine_diff_density_min         -1.605
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Flack x determined using 6561 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.056(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         16398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+0.2410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0591
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                15611
_reflns_number_total             16398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02122_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_formula_sum        'C33 H51 Cl2 N2 O2 Re1'
_cod_database_code               4349232
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.685
_shelx_estimated_absorpt_t_max   0.956
_shelx_res_checksum              44951
_shelx_hkl_checksum              86014