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_7059465
_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 Cl4 N4 O4 P2 Re2, 2(C3 H6 O)'
_chemical_formula_sum            'C56 H58 Cl4 N4 O6 P2 Re2'
_chemical_formula_weight         1459.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-25 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.7280(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.75942(9)
_cell_length_b                   14.22970(7)
_cell_length_c                   25.43850(12)
_cell_measurement_reflns_used    92892
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      78.7640
_cell_measurement_theta_min      3.5350
_cell_volume                     5638.57(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.16c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.16c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.16c (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      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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    -62.00 -37.00   0.50    0.34    --  -50.71 -52.00 -90.00   50
  2  \w   -105.00 -38.00   0.50    0.34    --  -50.71 -50.00  75.99  134
  3  \w   -127.00 -73.00   0.50    0.34    --  -50.71 -38.00  30.00  108
  4  \w    -91.00 -50.00   0.50    1.36    --  -86.25  56.00-109.27   82
  5  \w   -127.00 -41.00   0.50    0.34    --  -50.71 -42.00 -40.45  172
  6  \w   -122.00 -96.00   0.50    0.34    --  -50.71 -52.00 -90.00   52
  7  \w     62.00  88.00   0.50    0.34    --   50.71  57.00-150.00   52
  8  \w     31.00 108.00   0.50    1.36    --  107.75 -15.00 -90.00  154
  9  \w    122.00 175.00   0.50    1.36    --  107.75  15.00 -30.00  106
 10  \w    149.00 175.00   0.50    1.36    --  107.75  52.00  55.00   52
 11  \w    128.00 154.00   0.50    1.36    --  107.75  15.00   0.00   52
 12  \w    124.00 150.00   0.50    1.36    --  107.75  15.00  30.00   52
 13  \w    109.00 142.00   0.50    1.36    --  107.75  52.00  55.00   66
 14  \w    104.00 132.00   0.50    1.36    --  107.75  47.00 142.39   56
 15  \w     68.00  93.00   0.50    1.36    --  107.75  -4.00  24.41   50
 16  \w     95.00 120.00   0.50    1.36    --  107.75  15.00   0.00   50
 17  \w     69.00  94.00   0.50    1.36    --  107.75  -5.00  93.08   50
 18  \w     63.00 108.00   0.50    1.36    --  107.75 -15.00  90.00   90
 19  \w     52.00  78.00   0.50    1.36    --  107.75 -59.00 111.74   52
 20  \w     61.00  96.00   0.50    1.36    --  107.75 -58.00 136.98   70
 21  \w     54.00 100.00   0.50    1.36    --  107.75 -59.00  78.08   92
 22  \w     44.00  69.00   0.50    1.36    --  107.75 -30.00  30.00   50
 23  \w     42.00 102.00   0.50    1.36    --  107.75 -59.00  21.98  120
 24  \w     49.00  75.00   0.50    1.36    --  107.75 -45.00  53.10   52
 25  \w     35.00  87.00   0.50    1.36    --  107.75 -57.00  -1.78  104
 26  \w     32.00  58.00   0.50    1.36    --  107.75 -45.00 -90.00   52
 27  \w     51.00  76.00   0.50    1.36    --  107.75 -45.00-120.00   50
 28  \w     48.00  77.00   0.50    1.36    --  107.75 -45.00-150.00   58
 29  \w     34.00  85.00   0.50    1.36    --  107.75 -53.00-176.74  102
 30  \w     39.00  68.00   0.50    1.36    --  107.75 -48.00-123.78   58
 31  \w     39.00  80.00   0.50    1.36    --  107.75 -57.00 -60.14   82
 32  \w     32.00  61.00   0.50    1.36    --  107.75 -45.00 -60.00   58
 33  \w     35.00  69.00   0.50    1.36    --  107.75 -55.00 -27.82   68
 34  \w     28.00  61.00   0.50    1.36    --  107.75  -4.00  24.41   66
 35  \w     35.00  61.00   0.50    1.36    --  107.75 -48.00  20.90   52
 36  \w     36.00  61.00   0.50    1.36    --  107.75 -58.00  56.23   50
 37  \w     30.00  55.00   0.50    1.36    --  107.75 -38.00 101.98   50
 38  \w     45.00  77.00   0.50    1.36    --  107.75 -59.00 123.92   64
 39  \w     35.00  69.00   0.50    1.36    --  107.75 -30.00 120.00   68
 40  \w     29.00  59.00   0.50    1.36    --  107.75 -15.00  90.00   60
 41  \w     33.00  58.00   0.50    1.36    --  107.75 -52.00 128.51   50
 42  \w     36.00  85.00   0.50    1.36    --  107.75 -55.00 142.39   98
 43  \w     37.00  63.00   0.50    1.36    --  107.75 -56.00  59.65   52
 44  \w     30.00  62.00   0.50    1.36    --  107.75 -30.00 -30.00   64
 45  \w     31.00  65.00   0.50    1.36    --  107.75 -30.00 -60.00   68
 46  \w     31.00  69.00   0.50    1.36    --  107.75 -30.00-120.00   76
 47  \w     29.00  54.00   0.50    1.36    --  107.75 -30.00-180.00   50
 48  \w    -73.00 -37.00   0.50    0.34    --  -50.71 -57.00 150.00   72
 49  \w    -18.00  27.00   0.50    0.34    --  -50.71  19.00  60.00   90
 50  \w    -63.00 -26.00   0.50    0.34    --  -50.71  19.00  60.00   74
 51  \w   -116.00 -79.00   0.50    0.34    --  -50.71 -57.00-180.00   74
 52  \w    -71.00 -41.00   0.50    0.34    --  -50.71 -57.00-180.00   60
 53  \w      7.00  63.00   0.50    0.34    --   50.71 -19.00 150.00  112
 54  \w     13.00  44.00   0.50    0.34    --   50.71 -57.00-120.00   62
 55  \w    -98.00 -72.00   0.50    1.36    --  -86.25 -60.00 179.49   52
 56  \w    -99.00 -73.00   0.50    1.36    --  -86.25 -59.00 144.33   52
 57  \w   -100.00 -71.00   0.50    1.36    --  -86.25 -59.00 115.15   58
 58  \w    -96.00 -71.00   0.50    1.36    --  -86.25 -56.00 146.70   50
 59  \w     95.00 121.00   0.50    1.36    --  107.75  45.00-150.00   52
 60  \w    112.00 138.00   0.50    1.36    --  107.75  59.00 156.25   52
 61  \w     96.00 145.00   0.50    1.36    --  107.75  45.00 120.00   98
 62  \w     59.00  98.00   0.50    1.36    --  107.75 -59.00 -47.67   78
 63  \w     96.00 134.00   0.50    1.36    --  107.75  48.00  87.87   76
 64  \w    100.00 161.00   0.50    1.36    --  107.75  55.00-155.15  122
 65  \w    121.00 177.00   0.50    1.36    --  107.75  40.00-176.84  112
 66  \w     96.00 133.00   0.50    1.36    --  107.75  38.00  -0.08   74
 67  \w    103.00 130.00   0.50    1.36    --  107.75  51.00 -94.44   54
 68  \w     95.00 159.00   0.50    1.36    --  107.75  45.00 150.00  128
 69  \w     92.00 117.00   0.50    1.36    --  107.75  60.00-156.92   50
 70  \w     29.00  54.00   0.50    1.36    --  107.75 -30.00   0.00   50
 71  \w     94.00 131.00   0.50    1.36    --  107.75  45.00-120.00   74
 72  \w     97.00 123.00   0.50    1.36    --  107.75  30.00  90.00   52
 73  \w    142.00 171.00   0.50    1.36    --  107.75  15.00 120.00   58
 74  \w     94.00 123.00   0.50    1.36    --  107.75  30.00-150.00   58
 75  \w     76.00 102.00   0.50    1.36    --  107.75 -59.00 -28.39   52
 76  \w    101.00 156.00   0.50    1.36    --  107.75  51.00   6.34  110
 77  \w     93.00 135.00   0.50    1.36    --  107.75  58.00 -56.60   84
 78  \w    153.00 178.00   0.50    1.36    --  107.75  59.00 153.79   50
 79  \w     40.00  66.00   0.50    1.36    --  107.75 -30.00 -30.00   52
 80  \w     63.00  89.00   0.50    1.36    --  107.75 -56.00-119.70   52
 81  \w    151.00 178.00   0.50    1.36    --  107.75  30.00  60.00   54
 82  \w    102.00 139.00   0.50    1.36    --  107.75  60.00-121.64   74
 83  \w     94.00 122.00   0.50    1.36    --  107.75  30.00  60.00   56
 84  \w    132.00 175.00   0.50    1.36    --  107.75  21.00 132.74   86
 85  \w     53.00  96.00   0.50    1.36    --  107.75 -59.00 -77.88   86
 86  \w     94.00 120.00   0.50    1.36    --  107.75  45.00  30.00   52
 87  \w    147.00 173.00   0.50    1.36    --  107.75  30.00-180.00   52
 88  \w     95.00 133.00   0.50    1.36    --  107.75  51.00-113.38   76
 89  \w     48.00  74.00   0.50    1.36    --  107.75 -15.00  60.00   52
 90  \w     79.00 105.00   0.50    1.36    --  107.75  -5.00-152.16   52
 91  \w     39.00  65.00   0.50    1.36    --  107.75 -55.00 -45.06   52
 92  \w     73.00  99.00   0.50    1.36    --  107.75 -58.00 163.70   52
 93  \w     51.00  77.00   0.50    1.36    --  107.75 -59.00  -6.98   52
 94  \w    102.00 129.00   0.50    1.36    --  107.75  45.00  60.00   54
 95  \w    138.00 171.00   0.50    1.36    --  107.75  45.00  90.00   66
 96  \w    118.00 144.00   0.50    1.36    --  107.75  30.00-120.00   52
 97  \w    111.00 137.00   0.50    1.36    --  107.75  30.00   0.00   52
 98  \w     92.00 117.00   0.50    1.36    --  107.75  59.00 153.79   50
 99  \w    103.00 129.00   0.50    1.36    --  107.75  58.00 117.40   52
100  \w     94.00 148.00   0.50    1.36    --  107.75  52.00 158.83  108
;
_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      -0.0104029000
_diffrn_orient_matrix_UB_12      0.0649723000
_diffrn_orient_matrix_UB_13      -0.0490078000
_diffrn_orient_matrix_UB_21      0.0933488000
_diffrn_orient_matrix_UB_22      -0.0206961000
_diffrn_orient_matrix_UB_23      -0.0075701000
_diffrn_orient_matrix_UB_31      -0.0309753000
_diffrn_orient_matrix_UB_32      -0.0841058000
_diffrn_orient_matrix_UB_33      -0.0360172000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            26976
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.933
_diffrn_reflns_theta_min         3.102
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.975
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.16c (Rigaku Oxford Diffraction, 2018)
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    1.719
_exptl_crystal_description       prism
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.047
_refine_diff_density_max         1.331
_refine_diff_density_min         -1.785
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         26976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+2.9329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26250
_reflns_number_total             26976
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 5.0793\% 
 around [-0.87 0.45 0.20] (reciprocal) or [-0.84 0.54 -0.00] (direct)
;
_cod_data_source_file            d0nj00182a2.cif
_cod_data_source_block           jm181030_17_twin1_hklf5
_cod_depositor_comments
;Adding full bibliography for 7059464--7059466.cif.

 Adding full bibliography for 7059464--7059466.cif.
;
_cod_database_code               7059465
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Re2 Cl4 N4 O6 P2 C60 H50'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5132(5)
 0.4868(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C10(H10), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C52(H52), C53(H53),
  C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C82(H82), C83(H83),
  C84(H84), C85(H85), C86(H86)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C13(H13B,H13A,H13C), C14(H14A,H14B,H14C),
 C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C95(H95A,H95B,H95C), C96(H96A,H96B,
 H96C)
;
_shelx_res_checksum              2779
_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 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.794
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2