The reaction of oxidorhenium(v) with dipodal and tripodal aroylhydrazines: formation of dinuclear and trinuclear aroylhydrazone-bridged rhenium(v) complexes
Mukiza, Janvier; Blacque, Olivier; Habarurema, Gratien; Kampire, Edwige; New Journal of Chemistry 44 (2020) 7080–7090; doi:10.1039/D0NJ00182A

data_7059464
_publ_section_title
;
 The reaction of oxidorhenium(v) with dipodal and tripodal
 aroylhydrazines: formation of dinuclear and trinuclear
 aroylhydrazone-bridged rhenium(v) complexes
;
_journal_issue                   17
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7080
_journal_page_last               7090
_journal_paper_doi               10.1039/D0NJ00182A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C50 H46 Br4 N4 O4 P2 Re2, 2(C H2 Cl2)'
_chemical_formula_sum            'C52 H50 Br4 Cl4 N4 O4 P2 Re2'
_chemical_formula_weight         1690.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-24 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.9820(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.55266(16)
_cell_length_b                   14.23673(6)
_cell_length_c                   16.34599(10)
_cell_measurement_reflns_used    43877
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      78.5610
_cell_measurement_theta_min      3.5720
_cell_volume                     5744.31(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      159.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -60.00 -15.00   0.50    1.50    --  -50.46  57.00 -30.00   90
  2  \w    -66.00  -1.00   0.50    1.50    --  -50.46  57.00-180.00  130
  3  \w    -84.00 -37.00   0.50    1.50    --  -50.46 -57.00 -60.00   94
  4  \w    -63.00 -35.00   0.50    1.50    --  -50.46 -57.00   0.00   56
  5  \w    -74.00 -35.00   0.50    1.50    --  -50.46 -57.00 -30.00   78
  6  \w   -105.00 -36.00   0.50    1.50    --  -50.46 -57.00-150.00  138
  7  \w     35.00  61.00   0.50    1.50    --   50.46  58.00 -53.66   52
  8  \w    118.00 175.00   0.50    6.00    --  107.75  15.00  30.00  114
  9  \w    149.00 178.00   0.50    6.00    --  107.75  45.00  90.00   58
 10  \w     95.00 139.00   0.50    6.00    --  107.75  45.00  90.00   88
 11  \w    103.00 129.00   0.50    6.00    --  107.75  15.00  90.00   52
 12  \w     87.00 119.00   0.50    6.00    --  107.75 -15.00   0.00   64
 13  \w     72.00  99.00   0.50    6.00    --  107.75 -60.00 -69.45   54
 14  \w     74.00 100.00   0.50    6.00    --  107.75 -59.00-100.62   52
 15  \w     75.00 100.00   0.50    6.00    --  107.75 -59.00-141.14   50
 16  \w     70.00  99.00   0.50    6.00    --  107.75 -59.00-156.95   58
 17  \w    108.00 138.00   0.50    6.00    --  107.75  15.00 -90.00   60
 18  \w    117.00 177.00   0.50    6.00    --  107.75  57.00-179.15  120
 19  \w     57.00 102.00   0.50    6.00    --  107.75 -59.00 -10.37   90
 20  \w     40.00  74.00   0.50    6.00    --  107.75 -56.00  54.37   68
 21  \w     40.00  65.00   0.50    6.00    --  107.75 -15.00   0.00   50
 22  \w     37.00 113.00   0.50    6.00    --  107.75 -60.00 -44.80  152
 23  \w     38.00  67.00   0.50    6.00    --  107.75 -59.00-156.95   58
 24  \w     42.00  95.00   0.50    6.00    --  107.75 -60.00-124.28  106
 25  \w     30.00  65.00   0.50    6.00    --  107.75 -30.00-120.00   70
 26  \w     33.00  58.00   0.50    6.00    --  107.75 -51.00-145.07   50
 27  \w     38.00 101.00   0.50    6.00    --  107.75 -60.00  31.28  126
 28  \w     51.00  94.00   0.50    6.00    --  107.75 -11.00 116.84   86
 29  \w     58.00  96.00   0.50    6.00    --  107.75 -11.00 172.32   76
 30  \w     39.00  65.00   0.50    6.00    --  107.75 -56.00  90.34   52
 31  \w     36.00  84.00   0.50    6.00    --  107.75 -51.00 115.13   96
 32  \w     33.00  76.00   0.50    6.00    --  107.75 -45.00 150.00   86
 33  \w     30.00  63.00   0.50    6.00    --  107.75 -30.00 120.00   66
 34  \w   -121.00 -63.00   0.50    1.50    --  -50.46 -38.00 120.00  116
 35  \w    -64.00 -28.00   0.50    1.50    --  -50.46  57.00  60.00   72
 36  \w     38.00  87.00   0.50    1.50    --   50.46  57.00 120.00   98
 37  \w     90.00 117.00   0.50    1.50    --   50.46  59.00-153.09   54
 38  \w    -15.00  15.00   0.50    1.50    --   50.46 -38.00  90.00   60
 39  \w     41.00  66.00   0.50    1.50    --   50.46 -57.00-120.00   50
 40  \w     37.00  72.00   0.50    1.50    --   50.46  57.00   0.00   70
 41  \w     37.00  69.00   0.50    1.50    --   50.46  59.00 -27.70   64
 42  \w     36.00  80.00   0.50    1.50    --   50.46  59.00-153.09   88
 43  \w     77.00 103.00   0.50    1.50    --   50.46  57.00   0.00   52
 44  \w     16.00  42.00   0.50    1.50    --   50.46 -38.00  90.00   52
 45  \w     79.00 106.00   0.50    6.00    --  107.75 -60.00  41.12   54
 46  \w    133.00 178.00   0.50    6.00    --  107.75  45.00 120.00   90
 47  \w     44.00  71.00   0.50    6.00    --  107.75 -45.00 -90.00   54
 48  \w     45.00  74.00   0.50    6.00    --  107.75 -45.00 -60.00   58
 49  \w    109.00 135.00   0.50    6.00    --  107.75  60.00   6.94   52
 50  \w     48.00  74.00   0.50    6.00    --  107.75 -60.00  41.12   52
 51  \w     62.00 111.00   0.50    6.00    --  107.75 -60.00 154.49   98
 52  \w     47.00  73.00   0.50    6.00    --  107.75 -15.00 -30.00   52
 53  \w     59.00 107.00   0.50    6.00    --  107.75 -60.00-170.24   96
 54  \w    132.00 165.00   0.50    6.00    --  107.75  32.00 -82.79   66
 55  \w     61.00  88.00   0.50    6.00    --  107.75 -60.00 131.99   54
 56  \w     95.00 120.00   0.50    6.00    --  107.75 -15.00 -30.00   50
 57  \w     98.00 147.00   0.50    6.00    --  107.75  30.00 120.00   98
 58  \w    143.00 170.00   0.50    6.00    --  107.75  60.00   6.94   54
 59  \w     35.00  86.00   0.50    6.00    --  107.75 -55.00 140.27  102
 60  \w     70.00 119.00   0.50    6.00    --  107.75 -60.00 112.60   98
 61  \w     38.00  82.00   0.50    6.00    --  107.75 -54.00  81.15   88
 62  \w     40.00  66.00   0.50    6.00    --  107.75 -15.00  90.00   52
 63  \w     89.00 115.00   0.50    6.00    --  107.75 -15.00  90.00   52
 64  \w     54.00  86.00   0.50    6.00    --  107.75 -17.00 -48.19   64
 65  \w     37.00  75.00   0.50    6.00    --  107.75 -45.00 -30.00   76
 66  \w     42.00  67.00   0.50    6.00    --  107.75 -45.00  30.00   50
 67  \w     32.00  57.00   0.50    6.00    --  107.75 -44.00 -18.40   50
 68  \w     31.00  56.00   0.50    6.00    --  107.75 -40.00 -89.21   50
 69  \w     94.00 124.00   0.50    6.00    --  107.75  30.00 -30.00   60
 70  \w    112.00 138.00   0.50    6.00    --  107.75  30.00 -90.00   52
 71  \w     54.00  81.00   0.50    6.00    --  107.75 -56.00 108.65   54
 72  \w     96.00 134.00   0.50    6.00    --  107.75  36.00 169.00   76
 73  \w    115.00 141.00   0.50    6.00    --  107.75  15.00 -30.00   52
 74  \w     29.00  54.00   0.50    6.00    --  107.75 -30.00 -90.00   50
 75  \w     36.00  77.00   0.50    6.00    --  107.75 -45.00-120.00   82
 76  \w     63.00 112.00   0.50    6.00    --  107.75  -9.00-110.26   98
 77  \w     52.00  94.00   0.50    6.00    --  107.75 -60.00  24.85   84
 78  \w     66.00 105.00   0.50    6.00    --  107.75 -60.00  71.43   78
 79  \w     54.00  81.00   0.50    6.00    --  107.75 -60.00 124.65   54
 80  \w    106.00 132.00   0.50    6.00    --  107.75  52.00 -16.69   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0009218000
_diffrn_orient_matrix_UB_12      0.1081696000
_diffrn_orient_matrix_UB_13      0.0012571000
_diffrn_orient_matrix_UB_21      -0.0289980000
_diffrn_orient_matrix_UB_22      -0.0001683000
_diffrn_orient_matrix_UB_23      0.0717554000
_diffrn_orient_matrix_UB_31      0.0552697000
_diffrn_orient_matrix_UB_32      -0.0019155000
_diffrn_orient_matrix_UB_33      0.0660930000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            58265
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.849
_diffrn_reflns_theta_min         3.581
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.992
_exptl_absorpt_correction_T_max  0.610
_exptl_absorpt_correction_T_min  0.347
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_description       plate
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.679
_refine_diff_density_min         -1.655
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5778
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0514P)^2^+45.9783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5596
_reflns_number_total             5778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00182a2.cif
_cod_data_source_block           jm181113_jmrevbrbhz2
_cod_depositor_comments
;Adding full bibliography for 7059464--7059466.cif.

 Adding full bibliography for 7059464--7059466.cif.
;
_cod_database_code               7059464
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C26 H22 Br2 Cl2 N2 O2 P Re'
_reflns_odcompleteness_completeness 91.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     79.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl43-C41B \\sim Cl44-C41B \\sim Cl41-C41 \\sim Cl42-C41
 with sigma of 0.02
 Cl43-Cl44 \\sim Cl42-Cl41
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl41 \\sim Cl44: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Cl42 \\sim Cl43: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
4. Rigid body (RIGU) restrains
 Cl42, C41, Cl41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl43)=Sof(Cl44)=Sof(C41B)=Sof(H41C)=Sof(H41D)=1-FVAR(1)
 Sof(Cl41)=Sof(Cl42)=Sof(C41)=Sof(H41A)=Sof(H41B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C41B(H41C,H41D)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34),
  C35(H35), C36(H36)
6.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              15524
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.303
_oxdiff_exptl_absorpt_empirical_full_min 0.752