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_7009020
_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            'C60 H82 Mn2 N8 Na2 O5'
_chemical_formula_weight         1151.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00(0)
_cell_angle_beta                 107.71(3)
_cell_angle_gamma                90.00(0)
_cell_formula_units_Z            2.00
_cell_length_a                   10.593(3)
_cell_length_b                   19.228(5)
_cell_length_c                   15.663(5)
_cell_measurement_reflns_used    143
_cell_measurement_temperature    25
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      20.2
_cell_volume                     3039.1(16)
_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           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_sigmaI/netI    0.2441
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7343
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0.8
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.4624
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.2580
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             1220.0
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.955
_refine_ls_goodness_of_fit_obs   1.199
_refine_ls_hydrogen_treatment    not_refined
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5158
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.157
_refine_ls_restrained_S_obs      1.201
_refine_ls_R_factor_all          0.2783
_refine_ls_R_factor_obs          0.0641
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2877
_refine_ls_wR_factor_obs         0.1598
_reflns_number_observed          2119
_reflns_number_total             6977
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908121f.txt
_cod_data_source_block           COMPLEX_8
_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^)+(0.1069P)^2^+0.0000P] 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^)+(0.1069P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3039.(2)
_cod_original_sg_symbol_H-M      P21/N
_cod_original_formula_sum        C60H82Mn2N8Na2O5
_cod_database_code               7009020