Crystal and molecular structures of <i>fac</i>-[Re(Bid)(PPh~3~)(CO)~3~] [Bid is tropolone (TropH) and tribromotropolone (TropBr~3~H)]
Schutte-Smith, Marietjie; Visser, Hendrik Gideon; Acta Crystallographica Section C 78 (2022) –; doi:10.1107/S205322962200465X

data_2022611
_publ_section_title
;
 Crystal and molecular structures of <i>fac</i>-[Re(Bid)(PPh~3~)(CO)~3~]
 [Bid is tropolone (TropH) and tribromotropolone (TropBr~3~H)]
;
_journal_coeditor_code           OC3014
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205322962200465X
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Re (C7 H2 Br3 O2) (C18 H15 P) (C O)3]'
_chemical_formula_moiety         'C28 H17 Br3 O5 P Re'
_chemical_formula_sum            'C28 H17 Br3 O5 P Re'
_chemical_formula_weight         890.32
_chemical_name_systematic
<i>fac</i>-Tricarbonyl(3,5,7-tribromotropolonato-\k^2^<i>O</i>,<i>O</i>')(triphenylphosphane-\k<i>P</i>)rhenium(I)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                102.221(5)
_cell_angle_beta                 93.891(5)
_cell_angle_gamma                109.093(5)
_cell_formula_units_Z            2
_cell_length_a                   8.5413(12)
_cell_length_b                   8.7024(13)
_cell_length_c                   20.376(3)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.55
_cell_volume                     1383.3(4)
_computing_cell_refinement
;
<i>SAINT-Plus</i> (Bruker, 2012)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2012)
;
_computing_data_reduction
;
<i>SAINT-Plus</i> (Bruker, 2012)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2019)
;
_computing_publication_material
;
<i>WinGX</i> (Farrugia, 2012) and <i>DIAMOND</i> (Brandenburg & Putz,
2019)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      104(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.331
_diffrn_reflns_theta_min         2.068
_exptl_absorpt_coefficient_mu    8.820
_exptl_absorpt_correction_T_max  0.728
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.138
_exptl_crystal_description       stout
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.932
_refine_diff_density_min         -1.485
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0288
_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^)+2.6793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                5913
_reflns_number_total             6818
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oc3014sup1.cif
_cod_data_source_block           2
_cod_original_cell_volume        1383.3(3)
_cod_database_code               2022611
_shelx_estimated_absorpt_t_min   0.306
_shelx_estimated_absorpt_t_max   0.742
_shelx_hkl_checksum              96815
_shelx_res_checksum              72110
_cod_database_fobs_code 2022611