Pyrazolone-based nitrido complexes: synthesis and nitrogen transfer to alkenes
Fredy R. Pérez; Julio Belmar; Yanko Moreno; Ricardo Baggio; Octavio Peña; New Journal of Chemistry 29 (2005) 283–; doi:10.1039/b415101a

data_7050056
_publ_section_title
;
 Pyrazolone-based nitrido complexes: synthesis and nitrogen transfer to
 alkenes
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              283
_journal_paper_doi               10.1039/b415101a
_journal_volume                  29
_journal_year                    2005
_chemical_formula_moiety         'C28 H48 Mn N7 O2'
_chemical_formula_sum            'C28 H48 Mn N7 O2'
_chemical_formula_weight         569.67
_chemical_name_systematic
;
N,N'-Bis-{[1-(n-hexyl)-3-methyl-5-oxo-2-pyrazolin-4-ilpropyliden]-1-yl}
ethylenedi-amino  manganese(V)
;
_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                113.953(3)
_cell_angle_beta                 90.227(2)
_cell_angle_gamma                102.320(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2780(11)
_cell_length_b                   13.5310(16)
_cell_length_c                   13.9489(17)
_cell_measurement_reflns_used    831
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      48.74
_cell_measurement_theta_min      4.98
_cell_volume                     1555.4(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.062
_diffrn_reflns_av_sigmaI/netI    0.048
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9221
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.78
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SAINT/SADABS (Bruker, 2000)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6483
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0947P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1961
_reflns_number_gt                3338
_reflns_number_total             6483
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b415101a.txt
_cod_data_source_block           Mn_Cmplx
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050056