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_7059466
_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
; 0.903(C72 H66 Br4.29 Cl1.71 N6 O6 P3 Re3)
, 0.097(C54 H52 Br2.85 Cl1.15 N6 O5 P2 Re2)
, 3(C3 H6 O)
;
_chemical_formula_sum
'C79.25 H82.64 Br4.15 Cl1.65 N6 O8.9 P2.9 Re2.9'
_chemical_formula_weight         2282.28
_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   mixed
_audit_creation_date             2020-02-28
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-03-22 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.356(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7456(5)
_cell_length_b                   15.7521(4)
_cell_length_c                   26.8070(7)
_cell_measurement_reflns_used    42156
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      29.4060
_cell_measurement_theta_min      2.5030
_cell_volume                     8286.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -25.00  29.40   0.80   40.00    --  -10.12 -99.00 150.00   68
  2  \w    -84.00  20.00   0.80   40.00    --  -10.12 -77.00 -90.00  130
  3  \w    -83.00  11.40   0.80   40.00    --  -10.12 -38.00   0.00  118
  4  \w    -25.00  51.00   0.80   40.00    --   10.74 -99.00 -30.00   95
  5  \w    -12.00  82.40   0.80   40.00    --   10.74  38.00-150.00  118
  6  \w    -62.00  32.40   0.80   40.00    --   10.74 -38.00 -90.00  118
  7  \w    -25.00  43.00   0.80   40.00    --   10.74 -99.00 120.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0272947000
_diffrn_orient_matrix_UB_12      -0.0170893000
_diffrn_orient_matrix_UB_13      0.0119009000
_diffrn_orient_matrix_UB_21      0.0232453000
_diffrn_orient_matrix_UB_22      -0.0265266000
_diffrn_orient_matrix_UB_23      0.0148540000
_diffrn_orient_matrix_UB_31      0.0046711000
_diffrn_orient_matrix_UB_32      0.0320993000
_diffrn_orient_matrix_UB_33      0.0186283000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            126205
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.176
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.398
_exptl_absorpt_correction_T_max  0.533
_exptl_absorpt_correction_T_min  0.255
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_description       block
_exptl_crystal_F_000             4424
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.485
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         15163
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0351P)^2^+10.5760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13137
_reflns_number_total             15163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00182a2.cif
_cod_data_source_block           CCDC1955881
_cod_depositor_comments
;Adding full bibliography for 7059464--7059466.cif.

 Adding full bibliography for 7059464--7059466.cif.
;
_cod_original_cell_volume        8286.6(4)
_cod_original_formula_sum
'C79.25 H82.64 Br4.15 Cl1.65 N6 O8.90 P2.90 Re2.90'
_cod_database_code               7059466
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.490
_shelx_estimated_absorpt_t_min   0.227
_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, All O(H) groups
2. Restrained distances
 Re1-Cl1A = Re1-Cl1B = Re3-Cl3A = Re3-Cl3B = Re2-Cl2A = Re2-Cl2B
 2.47 with sigma of 0.005
 Re1-Br1B = Re1-Br1A = Re2-Br2B = Re2-Br2A = Re3-Br3B = Re3-Br3A
 2.5 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Br2A \\sim Br2B \\sim Cl2A \\sim Cl2B: within 3A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 3A
Br1A \\sim Br1B \\sim Cl1A \\sim Cl1B: within 3A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 3A
Br3A \\sim Br3B \\sim Cl3A \\sim Cl3B: within 3A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 3A
N3 \\sim C48 \\sim C49 \\sim C50: within 3A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 3A
4. Others
 Sof(Cl1A)=0.90328*(1-FVAR(2))
 Sof(Br1B)=0.90328*FVAR(2)
 Sof(Cl1B)=0.90328*(1-FVAR(3))
 Sof(Br1A)=0.90328*FVAR(3)
 Sof(Cl3B)=1-FVAR(3)
 Sof(Br3A)=FVAR(3)
 Sof(Cl3A)=1-FVAR(4)
 Sof(Br3B)=FVAR(4)
 Sof(Br2A)=1-FVAR(5)
 Sof(Cl2B)=FVAR(5)
 Sof(Br2B)=1-FVAR(6)
 Sof(Cl2A)=FVAR(6)
 Sof(H4A)=1-FVAR(7)
 Sof(C30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=
 Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=
 Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(C43)=
 Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=
 Sof(H47)=Sof(O3)=Sof(P2)=Sof(Re1)=FVAR(7)
 Fixed X: H4A(0.36662)
 Fixed Y: H4A(0.46731)
 Fixed Z: H4A(0.426449)
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), C24(H24), C26(H26),
  C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C37(H37),
 C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46),
  C47(H47), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C59(H59),
 C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66), C67(H67), C68(H68),
  C69(H69)
5.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C)
;
_shelx_res_checksum              61915
_shelx_fab_checksum              34606
_platon_squeeze_void_probe_radius 1.20