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_7038270
_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 Br N2 O2 P2 Re, C18 H15 P, F6 P'
_chemical_formula_sum            'C74 H60 Br F6 N2 O2 P4 Re'
_chemical_formula_weight         1513.23
_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                99.237(2)
_cell_angle_beta                 107.373(2)
_cell_angle_gamma                108.801(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8734(3)
_cell_length_b                   17.2825(5)
_cell_length_c                   18.3204(5)
_cell_measurement_reflns_used    11825
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1460
_cell_measurement_theta_min      3.6420
_cell_volume                     3256.41(18)
_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  0.0647
_diffrn_reflns_av_unetI/netI     0.0855
_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       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30772
_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         3.345
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.644
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61863
_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    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1516
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.099
_refine_diff_density_max         1.714
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         11445
_refine_ls_number_restraints     501
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.1991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9333
_reflns_number_total             11445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03598h2.cif
_cod_data_source_block           ren383
_cod_original_cell_volume        3256.39(17)
_cod_database_code               7038270
_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
 P3-C69 \\sim P3A-C69 \\sim P3A-C63 \\sim P3-C63 \\sim P3A-C57A \\sim P3-C57
 with sigma of 0.01
 P4-F2A \\sim P4-F2 \\sim P4-F3A \\sim P4-F3 \\sim P4-F5A \\sim P4-F5 \\sim
P4-F6A \\sim P4-F6 \\sim P4-F1A ~
 P4-F1 \\sim P4-F4A \\sim P4-F4
 with sigma of 0.005
 F1A-F2A \\sim F1A-F4A \\sim F1A-F5A \\sim F1A-F6A \\sim F3A-F2A \\sim F3A-F4A
\\sim F3A-F5A \\sim F3A-F6A
 \\sim F1-F2 \\sim F1-F4 \\sim F1-F5 \\sim F1-F6 \\sim F3-F2 \\sim F3-F4 \\sim
F3-F5 \\sim F3-F6
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
P3A \\sim P3: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006
C58 \\sim C59 \\sim C60 \\sim C61 \\sim C57A \\sim C58A \\sim C59A \\sim C60A
\\sim C61A \\sim C62A \\sim C57 \\sim C62: 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 F4A \\sim F3A \\sim F5A
\\sim F6A \\sim F1A \\sim F2A: within 2A with sigma of 0.003 and sigma for
terminal atoms of 0.006
4. Others
 Fixed Sof: P3(0.43256) C57(0.43256) C58(0.43256) H8BA(0.43256) C59(0.43256)
 H9BA(0.43256) C60(0.43256) H0CA(0.43256) C61(0.43256) H1CA(0.43256)
 C62(0.43256) H2CA(0.43256) F1(0.5) F2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5)
 F4A(0.5) F3A(0.5) F5A(0.5) F6A(0.5) F1A(0.5) F2A(0.5) C57A(0.56744)
 C58A(0.56744) H3DA(0.56744) C59A(0.56744) H4DA(0.56744) C60A(0.56744)
 H5DA(0.56744) C61A(0.56744) H6DA(0.56744) C62A(0.56744) H7DA(0.56744)
 P3A(0.56744)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H), C3(HA), C4(HB), C5(HC), C6(HD), C8(HE), C9(HF), C10(HG), C11(HH),
 C12(HI), C14(HJ), C15(HK), C16(HL), C17(HM), C18(HN), C20(HO), C21(HP),
 C22(HQ), C23(HR), C27(HS), C28(HT), C29(HU), C30(HV), C33(HW), C34(HX),
 C36(HY), C37(HZ), C40(H3AA), C41(H4AA), C42(H5AA), C43(H6AA), C44(H7AA),
 C46(H8AA), C47(H9AA), C48(H0BA), C49(H1BA), C50(H2BA), C52(H3BA), C53(H4BA),
 C54(H5BA), C55(H6BA), C56(H7BA), C58(H8BA), C59(H9BA), C60(H0CA), C61(H1CA),
 C62(H2CA), C64(H3CA), C65(H4CA), C66(H5CA), C67(H6CA), C68(H7CA), C70(H8CA),
 C71(H9CA), C72(H0DA), C73(H1DA), C74(H2DA), C58A(H3DA), C59A(H4DA), C60A(H5DA),
  C61A(H6DA), C62A(H7DA)
5.b Fitted hexagon refined as free rotating group:
 C57(C58,C59,C60,C61,C62), C57A(C58A,C59A,C60A,C61A,C62A)
5.c Idealised Me refined as rotating group:
 C38(H0AA,H1AA,H2AA)
;
_shelx_res_checksum              88386
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'