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_2022610
_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 H5 O2) (C18 H15 P) (C O)3]'
_chemical_formula_moiety         'C28 H20 O5 P Re'
_chemical_formula_sum            'C28 H20 O5 P Re'
_chemical_formula_weight         653.61
_chemical_name_systematic
<i>fac</i>-Tricarbonyl(triphenylphosphane-\k<i>P</i>)(tropolonato-\k^2^<i>O</i>,<i>O</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                80.948(3)
_cell_angle_beta                 71.899(3)
_cell_angle_gamma                88.682(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9301(11)
_cell_length_b                   10.1686(10)
_cell_length_c                   12.7882(14)
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.92
_cell_volume                     1211.6(2)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_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  0.0371
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25538
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         2.921
_exptl_absorpt_coefficient_mu    5.118
_exptl_absorpt_correction_T_max  0.511
_exptl_absorpt_correction_T_min  0.357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.131
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.596
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0152
_refine_ls_R_factor_gt           0.0149
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+0.7798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0376
_refine_ls_wR_factor_ref         0.0378
_reflns_number_gt                5726
_reflns_number_total             5820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oc3014sup1.cif
_cod_data_source_block           1
_cod_database_code               2022610
_shelx_estimated_absorpt_t_min   0.339
_shelx_estimated_absorpt_t_max   0.554
_shelx_hkl_checksum              69815
_shelx_res_checksum              38917
_cod_database_fobs_code 2022610