The reactivity of dibenzotetramethyltetraaza[14]annulene-Mn(II): functionalisation of manganese in a macrocyclic environment
Franceschi, Federico; Hesschenbrouck, Joëlle; Solari, Euro; Floriani, Carlo; Re, Nazzareno; Rizzoli, Corrado; Chiesi-Villa, Angiola; Journal of the Chemical Society, Dalton Transactions  (2000) 593–; doi:10.1039/a908121f

data_7009018
_publ_section_title
;
 The reactivity of dibenzotetramethyltetraaza[14]annulene-Mn(II):
 functionalisation of manganese in a macrocyclic environment
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              593
_journal_paper_doi               10.1039/a908121f
_journal_year                    2000
_chemical_formula_sum            'C54 H62 B Mn N4 O4'
_chemical_formula_weight         896.86
_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
_cell_angle_alpha                99.11(2)
_cell_angle_beta                 91.60(2)
_cell_angle_gamma                81.55(2)
_cell_formula_units_Z            2.00
_cell_length_a                   12.260(2)
_cell_length_b                   16.785(2)
_cell_length_c                   11.637(1)
_cell_measurement_reflns_used    143
_cell_measurement_temperature    25
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      18.3
_cell_volume                     2338.8(5)
_computing_cell_refinement       'TEXSAN Software'
_computing_data_collection       'TEXSAN Software'
_computing_data_reduction        'TEXSAN Software'
_computing_structure_refinement  'SHELXS-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-76 (Sheldrick, 1976)'
_diffrn_ambient_temperature      143
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       omega/2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         fine-focussealedtube
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1435
_diffrn_reflns_av_sigmaI/netI    0.0895
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8081
_diffrn_reflns_theta_max         70.11
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        3.2
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.6782
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   'North et al. 1968'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.2735
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             952.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.896
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.085
_refine_ls_goodness_of_fit_obs   1.175
_refine_ls_hydrogen_treatment    not_refined
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         6729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.355
_refine_ls_restrained_S_obs      1.175
_refine_ls_R_factor_all          0.1391
_refine_ls_R_factor_obs          0.0738
_refine_ls_shift/esd_max         0.061
_refine_ls_shift/esd_mean        0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1552P)^2^+0.1594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3055
_refine_ls_wR_factor_obs         0.2019
_reflns_number_observed          4553
_reflns_number_total             7633
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908121f.txt
_cod_data_source_block           COMPLEX_4B
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1552P)^2^+0.1594P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1552P)^2^+0.1594P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        C54H62BMnN4O4
_cod_database_code               7009018