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_7242285
_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         'C24 H30 Br N4 O2 Re, 1[C5H12]'
_chemical_formula_sum            'C29 H42 Br N4 O2 Re'
_chemical_formula_weight         744.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-01-18 deposited with the CCDC.	2021-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1687(3)
_cell_length_b                   17.1375(3)
_cell_length_c                   12.0964(2)
_cell_measurement_reflns_used    80065
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      68.47
_cell_measurement_theta_min      3.65
_cell_volume                     3144.50(10)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0095
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38203
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.651
_diffrn_reflns_theta_max         67.651
_diffrn_reflns_theta_min         5.342
_diffrn_source                   'Primux 100 micro'
_exptl_absorpt_coefficient_mu    9.278
_exptl_absorpt_correction_T_max  0.1519
_exptl_absorpt_correction_T_min  0.0521
_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. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1480
_exptl_crystal_recrystallization_method 'layering DCM and pentane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.747
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2838
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0234
_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^)+(0.0331P)^2^+3.8512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2806
_reflns_number_total             2838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra00514f2.cif
_cod_data_source_block           ks113-1_e
_cod_database_code               7242285
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.606
_shelx_estimated_absorpt_t_min   0.258
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
Uanis(C8A) = Uanis(C7) = Uanis(C7A) = Uanis(C9) = Uanis(C9A) = Uanis(C8)
3. Others
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
 Fixed Sof: Br1(0.5) O2(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C15(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C10(H10), C11(H11), C12(H12)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC),
 C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC), C13(H13A,H13B,H13C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99766
_shelx_fab_checksum              74674
_olex2_exptl_crystal_mounting_method 'mounted on loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'