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_4120273
_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            'C47 H67 B Cl Co Mg N8 O5'
_chemical_formula_weight         953.59
_chemical_name_systematic
; 
 [(NO)(Cl)Co(Medoen)Mg(Me3TACN)(H2O)]BPh4 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 120.603(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.695(3)
_cell_length_b                   11.5842(12)
_cell_length_c                   30.376(4)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.10
_cell_measurement_theta_min      2.20
_cell_volume                     9599.5(19)
_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 0.946
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            150910
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         37.37
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_T_min  0.8538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker-AXS, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         23710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+8.7221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                15157
_reflns_number_total             23710
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4053653_si_002_6.cif
_cod_data_source_block           chu44
_cod_original_cell_volume        9599.4(19)
_cod_database_code               4120273