p-Tolylimido rhenium(v) complexes with phenolate-based ligands: synthesis, X-ray studies and catalytic activity in oxidation with tert-butylhydroperoxide.
Gryca, Izabela; Machura, Barbara; Małecki, Jan Grzegorz; Kusz, Joachim; Shul'pina, Lidia S.; Ikonnikov, Nikolay S.; Shul'pin, Georgiy B.; Dalton transactions (Cambridge, England : 2003) 45 (2015) 334–351; doi:10.1039/c5dt03598h

data_7038272
_publ_section_title
;
 p-Tolylimido rhenium(v) complexes with phenolate-based ligands:
 synthesis, X-ray studies and catalytic activity in oxidation with
 tert-butylhydroperoxide.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              334
_journal_page_last               351
_journal_paper_doi               10.1039/c5dt03598h
_journal_volume                  45
_journal_year                    2015
_chemical_formula_moiety         'C56 H45 Cl N2 O2 P2 Re, C18 H15 P, F6 P'
_chemical_formula_sum            'C74 H60 Cl F6 N2 O2 P4 Re'
_chemical_formula_weight         1468.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.09.21 svn.r3230 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-04 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                99.156(4)
_cell_angle_beta                 107.652(5)
_cell_angle_gamma                108.436(4)
_cell_formula_units_Z            2
_cell_length_a                   11.7939(7)
_cell_length_b                   17.2730(7)
_cell_length_c                   18.3327(11)
_cell_measurement_reflns_used    6920
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.4880
_cell_measurement_theta_min      3.6430
_cell_volume                     3239.1(4)
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_unetI/netI     0.1188
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31414
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.363
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.082
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81737
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlis RED, (2005)
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.068
_refine_diff_density_max         2.190
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         11368
_refine_ls_number_restraints     613
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0651
_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^)+(0.0842P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7838
_reflns_number_total             11368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03598h2.cif
_cod_data_source_block           ren403
_cod_original_cell_volume        3239.1(3)
_cod_database_code               7038272
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P4-F1 \\sim P4-F1A \\sim P4-F3 \\sim P4-F2 \\sim P4-F6A \\sim P4-F6 \\sim
P4-F5A \\sim P4-F5 \\sim P4-F3A ~
 P4-F2A \\sim P4-F4 \\sim P4-F4A
 with sigma of 0.01
 F1A-F2A \\sim F1A-F3A \\sim F1A-F5A \\sim F1A-F6A \\sim F4A-F2A \\sim F4A-F3A
\\sim F4A-F5A \\sim F4A-F6A
 \\sim F1-F2 \\sim F1-F3 \\sim F1-F5 \\sim F1-F6 \\sim F4-F2 \\sim F4-F3 \\sim
F4-F5 \\sim F4-F6 \\sim F3A-F2A ~
 F3A-F5A \\sim F6A-F2A \\sim F5A-F3 \\sim F2-F3 \\sim F5-F6 \\sim F2-F5
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C59 \\sim C60 \\sim C61 \\sim C62 \\sim C62A \\sim C61A \\sim C60A \\sim C59A
\\sim C57 \\sim C58 \\sim C57A \\sim C58A: within 2A with sigma of 0.003 and
sigma for terminal atoms of 0.006
P3 \\sim P3A: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F1A \\sim F6A \\sim F5A
\\sim F2A \\sim F3A \\sim F4A: within 2A with sigma of 0.003 and sigma for
terminal atoms of 0.006
4. Others
 Fixed Sof: P3(0.5458) C57(0.5458) C58(0.5458) H58(0.5458) C59(0.5458)
 H59(0.5458) C60(0.5458) H60(0.5458) C61(0.5458) H61(0.5458) C62(0.5458)
 H62(0.5458) F1(0.5) F2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5) F1A(0.5) F6A(0.5)
 F5A(0.5) F2A(0.5) F3A(0.5) F4A(0.5) C57A(0.4542) C62A(0.4542) H62A(0.4542)
 C61A(0.4542) H61A(0.4542) C60A(0.4542) H60A(0.4542) C59A(0.4542) H59A(0.4542)
 C58A(0.4542) H58A(0.4542) P3A(0.4542)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33),
 C34(H34), C36(H36), C37(H37), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
  C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62),
  C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C70(H70), C71(H71),
 C72(H72), C73(H73), C74(H74), C62A(H62A), C61A(H61A), C60A(H60A), C59A(H59A),
 C58A(H58A)
5.b Fitted hexagon refined as free rotating group:
 C57(C58,C59,C60,C61,C62), C57A(C62A,C61A,C60A,C59A,C58A)
5.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C)
;
_shelx_res_checksum              21170
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'