Oxidorhenium(V) Complexes with Tetradentate Iminophenolate Ligands: Influence of Ligand Flexibility on the Coordination Motif and Oxygen-Atom-Transfer Activity.
Zwettler, Niklas; Schachner, Jörg A; Belaj, Ferdinand; Mösch-Zanetti, Nadia C; Inorganic chemistry 55 (2016) 5973–5982; doi:10.1021/acs.inorgchem.6b00466

data_4347681
_publ_section_title
;
 Oxidorhenium(V) Complexes with Tetradentate Iminophenolate Ligands:
 Influence of Ligand Flexibility on the Coordination Motif and
 Oxygen-Atom-Transfer Activity.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5973
_journal_page_last               5982
_journal_paper_doi               10.1021/acs.inorgchem.6b00466
_journal_volume                  55
_journal_year                    2016
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         'C35 H52 Cl N2 O3 Re'
_chemical_formula_sum            'C35 H52 Cl N2 O3 Re'
_chemical_formula_weight         770.43
_chemical_name_common
; chloro-2,2'-{(2,2-dimethylpropane-1,3-diyl)bis[nitrilo(E)me-
thylylidene]}bis(4,6-di-tert-butyl-phenolato)-oxo-rhenium(V)
;
_chemical_name_systematic
; chloro-2,2'-{(2,2-dimethylpropane-1,3-diyl)bis[nitrilo(E)me-
thylylidene]}bis(4,6-di-tert-butyl-benzenolato)-oxo-rhenium(V)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'
_cell_angle_alpha                90
_cell_angle_beta                 101.6019(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4474(5)
_cell_length_b                   11.7992(4)
_cell_length_c                   18.4902(5)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.84
_cell_volume                     3515.01(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35370
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    3.568
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.227
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         10249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0168
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+1.7454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0416
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9300
_reflns_number_total             10249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00466_si_002.cif
_cod_data_source_block           ZN68c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347681
_shelx_estimated_absorpt_t_min   0.469
_shelx_estimated_absorpt_t_max   0.566
_shelxl_version_number           2014/6
_shelx_res_checksum              17346
_shelx_hkl_checksum              86785