Kinetics and Mechanism of CO Exchange in fac-[MBr2(solvent)(CO)3](-) (M = Re, (99)Tc).
Frei, Angelo; Sidler, David; Mokolokolo, Pennie; Braband, Henrik; Fox, Thomas; Spingler, Bernhard; Roodt, Andreas; Alberto, Roger; Inorganic chemistry 55 (2016) 9352–9360; doi:10.1021/acs.inorgchem.6b01503

data_4348663
_publ_section_title
;
 Kinetics and Mechanism of CO Exchange in fac-[MBr2(solvent)(CO)3](-) (M =
 Re, (99)Tc).
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9352
_journal_page_last               9360
_journal_paper_doi               10.1021/acs.inorgchem.6b01503
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C20 H29 Br2 N2 O3 Re'
_chemical_formula_weight         691.47
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.971(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0878(8)
_cell_length_b                   8.7429(3)
_cell_length_c                   16.4010(7)
_cell_measurement_reflns_used    10670
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      31.988
_cell_measurement_theta_min      2.683
_cell_volume                     2421.85(19)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2014)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2014)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Xcalibur Ruby'
_diffrn_measurement_method       '\o oscillation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24578
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.891
_diffrn_reflns_theta_min         2.497
_exptl_absorpt_coefficient_mu    8.338
_exptl_absorpt_correction_T_max  0.372
_exptl_absorpt_correction_T_min  0.119
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
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            colourless
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.167
_refine_diff_density_min         -2.173
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         8212
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0250P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6495
_reflns_number_total             8212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01503_si_002.cif
_cod_data_source_block           afx070416
_cod_original_cell_volume        2421.84(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348663
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.135
_shelx_estimated_absorpt_t_max   0.331
_shelx_res_checksum              15121
_shelx_hkl_checksum              36977