Aerobically stable and substitutionally labile α-diimine rhenium dicarbonyl complexes
Schindler, Kevin; Crochet, Aurélien; Zobi, Fabio; RSC Advances 11 (2021) 7511–7520; doi:10.1039/D1RA00514F

data_7242283
_publ_section_title
;
 Aerobically stable and substitutionally labile \a-diimine rhenium
 dicarbonyl complexes
;
_journal_issue                   13
_journal_name_full               'RSC Advances'
_journal_page_first              7511
_journal_page_last               7520
_journal_paper_doi               10.1039/D1RA00514F
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         '2(C20 H24 Br2 N2 O2 Re), C H2 Cl2'
_chemical_formula_sum            'C41 H50 Br4 Cl2 N4 O4 Re2'
_chemical_formula_weight         1425.79
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-18 deposited with the CCDC.	2021-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.998(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9090(4)
_cell_length_b                   31.7496(12)
_cell_length_c                   12.5191(4)
_cell_measurement_reflns_used    20885
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      1.28
_cell_volume                     4978.7(3)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2009)'
_computing_data_collection       'X-Area (Stoe & Cie, 2009)'
_computing_data_reduction        'X-RED32(Stoe & Cie, 2009)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            52668
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.393
_diffrn_reflns_theta_min         1.283
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Stoe IPDS2'
_exptl_absorpt_coefficient_mu    8.216
_exptl_absorpt_correction_T_max  0.3713
_exptl_absorpt_correction_T_min  0.2232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_description       needle
_exptl_crystal_F_000             2720
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and pentane  by diffusion'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.902
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.00014(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         10032
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0521P)^2^+6.2207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5459
_reflns_number_total             10032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra00514f2.cif
_cod_data_source_block           ks2
_cod_database_code               7242283
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.084
_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. Uiso/Uaniso restraints and constraints
Uanis(C38) = Uanis(C38A) = Uanis(C35) = Uanis(C36) = Uanis(C36A) = Uanis(C37) =
Uanis(C37A)
Uanis(C34) = Uanis(C34A) = Uanis(C33) = Uanis(C33A) = Uanis(C32) = Uanis(C32A)
3. Rigid body (RIGU) restrains
 C41, Cl1, Cl2
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Others
 Sof(C36A)=Sof(HX)=Sof(HY)=Sof(HZ)=Sof(C37A)=Sof(H0AA)=Sof(H1AA)=Sof(H2AA)=
 Sof(C38A)=Sof(H3AA)=Sof(H4AA)=Sof(H5AA)=1-FVAR(1)
 Sof(C36)=Sof(HO)=Sof(HP)=Sof(HQ)=Sof(C37)=Sof(HR)=Sof(HS)=Sof(HT)=Sof(C38)=
 Sof(HU)=Sof(HV)=Sof(HW)=FVAR(1)
 Sof(C32A)=Sof(H8AA)=Sof(H9AA)=Sof(H0BA)=Sof(C33A)=Sof(H1BA)=Sof(H2BA)=
 Sof(H3BA)=Sof(C34A)=Sof(H4BA)=Sof(H5BA)=Sof(H6BA)=1-FVAR(2)
 Sof(C32)=Sof(HF)=Sof(HG)=Sof(HH)=Sof(C33)=Sof(HI)=Sof(HJ)=Sof(HK)=Sof(C34)=
 Sof(HL)=Sof(HM)=Sof(HN)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C41(H6AA,H7AA)
5.b Aromatic/amide H refined with riding coordinates:
 C21(H), C22(HA), C24(HB), C27(HC), C29(HD), C30(HE), C1(H1), C2(H2), C4(H4),
 C7(H7), C9(H9), C10(H10)
5.c Idealised Me refined as rotating group:
 C32(HF,HG,HH), C33(HI,HJ,HK), C34(HL,HM,HN), C36(HO,HP,HQ), C37(HR,HS,HT),
 C38(HU,HV,HW), C36A(HX,HY,HZ), C37A(H0AA,H1AA,H2AA), C38A(H3AA,H4AA,H5AA),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C32A(H8AA,H9AA,H0BA),
 C33A(H1BA,H2BA,H3BA), C34A(H4BA,H5BA,H6BA)
;
_shelx_res_checksum              22562
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop in oil'
_olex2_submission_original_sample_id KS2
_olex2_submission_special_instructions 'No special instructions were received'