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_4120271
_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            'C43 H57 B Cl0 Co Mg N8 O4'
_chemical_formula_weight         844.02
_chemical_name_systematic
; 
 [(mu-NO2)Co(Medoen)Mg(Me3TACN)]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                84.582(2)
_cell_angle_beta                 79.196(2)
_cell_angle_gamma                83.448(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6227(13)
_cell_length_b                   11.9467(14)
_cell_length_c                   15.4979(18)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      2.26
_cell_volume                     2094.1(4)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2007)'
_computing_data_collection       'Bruker SMART v5.054 (Bruker, 2007)'
_computing_data_reduction        'SAINT V7.68A (Bruker, 2007)'
_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 8.19
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker SMART 1000'
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54074
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.09
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.9064
_exptl_absorpt_correction_T_min  0.8432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker-AXS, 2001)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       chunk
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         10342
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+1.9286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1427
_reflns_number_gt                7671
_reflns_number_total             10342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4053653_si_002_4.cif
_cod_data_source_block           chu51
_cod_database_code               4120271