Synthesis, X-ray Structure, Electrochemical, and EPR Studies of a Pentacoordinated Mn(II) Tetramethylcyclam Complex
Christophe Bucher; Emmanuelle Duval; Jean-Michel Barbe; Jean-Noël Verpeaux; Christian Amatore; Roger Guilard; Laurent Le Pape; Jean-Marc Latour; S. Dahaoui; Claude Lecomte; Inorganic Chemistry 40 (2001) 5722–5726; doi:10.1021/ic001472h

data_4320368
_publ_section_title
;
 Synthesis, X-ray Structure, Electrochemical, and EPR Studies of a
 Pentacoordinated Mn(II) Tetramethylcyclam Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5722
_journal_page_last               5726
_journal_paper_doi               10.1021/ic001472h
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C40 H55 B Cl Mn N5'
_chemical_formula_weight         707.09
_chemical_name_common            MnTMC
_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                74.86(3)
_cell_angle_beta                 72.61(3)
_cell_angle_gamma                74.31(3)
_cell_formula_units_Z            2
_cell_length_a                   11.514(2)
_cell_length_b                   13.300(3)
_cell_length_c                   14.225(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     1962.4(8)
_computing_cell_refinement       Enraf-Nonius
_computing_data_collection       Enraf-Nonius
_computing_data_reduction        Enraf-Nonius
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'CAD4 Enraf Nonius'
_diffrn_measurement_method       '\w-2\q 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6205
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             754
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.244
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0994P)^2^+1.3267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1630
_refine_ls_wR_factor_ref         0.1730
_reflns_number_gt                5008
_reflns_number_total             6205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001472h.cif
_cod_data_source_block           MnTMC
_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_original_cell_volume        1962.4(7)
_cod_database_code               4320368