Selective Nitrite Reduction at Heterobimetallic CoMg Complexes
Christopher Uyeda; Jonas C. Peters; Journal of the American Chemical Society 135 (2013) 12023–12031; doi:10.1021/ja4053653

data_4120269
_publ_section_title
;
 Selective Nitrite Reduction at Heterobimetallic CoMg Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12023
_journal_page_last               12031
_journal_paper_doi               10.1021/ja4053653
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C69 H88 B Co Mg N7 O4 P'
_chemical_formula_weight         1204.48
_chemical_name_systematic
; 
 [(PPh3)Co(Medoen)Mg(Me3TACN)(THF)]BPh4  
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.512(3)
_cell_angle_beta                 99.587(3)
_cell_angle_gamma                100.736(3)
_cell_formula_units_Z            2
_cell_length_a                   13.7524(8)
_cell_length_b                   14.0032(8)
_cell_length_c                   17.5215(10)
_cell_measurement_reflns_used    9499
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.94
_cell_measurement_theta_min      2.21
_cell_volume                     3144.5(3)
_computing_cell_refinement       'SAINT-Plus v7.66A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2010.7-0 (Bruker-AXS, 2010)'
_computing_data_reduction        'SAINT-Plus v7.66A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            373636
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         45.37
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.8958
_exptl_absorpt_correction_T_min  0.8744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker-AXS, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         49450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+0.6144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                34064
_reflns_number_total             49450
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4053653_si_002_2.cif
_cod_data_source_block           chu40
_cod_database_code               4120269