Intramolecular C-C Bond Coupling of Nitriles to a Diimine Ligand in Group 7 Metal Tricarbonyl Complexes.
Yempally, Veeranna; Fan, Wai Yip; Arndtsen, Bruce A.; Bengali, Ashfaq A.; Inorganic chemistry 54 (2015) 11441–11449; doi:10.1021/acs.inorgchem.5b02087

data_4346763
_publ_section_title
;
 Intramolecular C-C Bond Coupling of Nitriles to a Diimine Ligand in Group
 7 Metal Tricarbonyl Complexes.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11441
_journal_page_last               11449
_journal_paper_doi               10.1021/acs.inorgchem.5b02087
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C25 H23 Cl4 F6 N3 O3 P Re'
_chemical_formula_weight         886.43
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.252(3)
_cell_length_b                   15.880(3)
_cell_length_c                   12.165(2)
_cell_measurement_temperature    110(2)
_cell_volume                     3139.6(10)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37812
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.464
_diffrn_reflns_theta_min         1.793
_exptl_absorpt_coefficient_mu    4.330
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.543
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.878
_refine_diff_density_min         -3.333
_refine_diff_density_rms         0.231
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.057(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         7956
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1045
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                6628
_reflns_number_total             7956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02087_si_009.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        3139.6(9)
_cod_database_code               4346763
_shelx_estimated_absorpt_t_min   0.202
_shelx_estimated_absorpt_t_max   0.625
_shelxl_version_number           2014/6
_shelx_res_checksum              92844
_shelx_hkl_checksum              48355