Mechanism for the Formation of Substituted Manganese(V) Cyanidonitrido Complexes: Crystallographic and Kinetic Study of the Substitution Reactions of trans-[MnN(H2O)(CN)4]2- with Monodentate Pyridine and Bidentate Pyridine-Carboxylate Ligands
Hendrik J. van der Westhuizen; Reinout Meijboom; Marietjie Schutte; Andreas Roodt; Inorganic Chemistry 49 (2010) 9599–9608; doi:10.1021/ic101274q

data_4316817
_publ_section_title
;
 Mechanism for the Formation of Substituted Manganese(V) Cyanidonitrido
 Complexes: Crystallographic and Kinetic Study of the Substitution
 Reactions of trans-[MnN(H2O)(CN)4]2- with Monodentate Pyridine and
 Bidentate Pyridine-Carboxylate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9599
_journal_page_last               9608
_journal_paper_doi               10.1021/ic101274q
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         '2(C24 H20 P), C10 H7 Mn N6, C6 H7 N'
_chemical_formula_sum            'C64 H54 Mn N7 P2'
_chemical_formula_weight         1038.02
_chemical_name_systematic
;
 ?
;
_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                93.878(3)
_cell_angle_beta                 91.339(3)
_cell_angle_gamma                105.962(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6059(12)
_cell_length_b                   11.6267(14)
_cell_length_c                   25.636(3)
_cell_measurement_reflns_used    794
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.68
_cell_measurement_theta_min      2.38
_cell_volume                     2743.8(6)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1999)'
_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_data_reduction        'SAINT-Plus and XPREP (Bruker, 1999)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Brendt, 2001)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART CCD 1K'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_sigmaI/netI    0.1804
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16514
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         0.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_meas      1.25
_exptl_crystal_density_method    'Flotation in benzene/diiodomethane'
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         10692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.1809
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0511P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1515
_reflns_number_gt                4598
_reflns_number_total             10692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101274q_si_002_1.cif
_cod_data_source_block           mn3pic
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4316817