Synthesis, Spectroscopy, and Electrochemistry of (α-Diimine)M(CO)3Br, M = Mn, Re, Complexes: Ligands Isoelectronic to Bipyridyl Show Differences in CO2 Reduction.
Vollmer, Matthew V.; Machan, Charles W.; Clark, Melissa L.; Antholine, William E.; Agarwal, Jay; Schaefer, 3rd, Henry F; Kubiak, Clifford P.; Walensky, Justin R.; Organometallics 34 (2014) 3–12; doi:10.1021/om500838z

data_4085012
_publ_section_title
;
 Synthesis, Spectroscopy, and Electrochemistry of (\a-Diimine)M(CO)3Br, M
 = Mn, Re, Complexes: Ligands Isoelectronic to Bipyridyl Show Differences
 in CO2 Reduction.
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              3
_journal_page_last               12
_journal_paper_doi               10.1021/om500838z
_journal_volume                  34
_journal_year                    2014
_chemical_formula_moiety         'C21 H14 Br F6 Mn N2 O3'
_chemical_formula_sum            'C21 H14 Br F6 Mn N2 O3'
_chemical_formula_weight         591.19
_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'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.995(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7363(4)
_cell_length_b                   15.4011(6)
_cell_length_c                   12.7722(5)
_cell_measurement_reflns_used    5390
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      2.2
_cell_volume                     2229.99(15)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16256
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.392
_diffrn_reflns_theta_min         2.115
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    2.460
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 G\"ottingen, Germany).
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0416P)^2^+0.5029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3739
_reflns_number_total             4545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500838z_si_003.cif
_cod_data_source_block           mncf3dab
_cod_depositor_comments
;Adding full bibliography for 4085006--4085014.cif.

 Adding full bibliography for 4085006--4085014.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4085012
_shelx_estimated_absorpt_t_min   0.578
_shelx_estimated_absorpt_t_max   0.709
_shelxl_version_number           2013-4