Titanium and manganese complexes supported by a xanthene-bridged bis(tripodal N2O2) ligand: isomerization, intramolecular hydrogen bonding and metal-binding ability.
Hirotsu, Masakazu; Kawamoto, Keisuke; Tanaka, Rika; Nagai, Yuji; Ueno, Keiji; Teki, Yoshio; Kinoshita, Isamu; Dalton transactions (Cambridge, England : 2003) 42 (2013) 12220–12227; doi:10.1039/c3dt51389k

data_7021794
_publ_section_title
;
 Titanium and manganese complexes supported by a xanthene-bridged
 bis(tripodal N2O2) ligand: isomerization, intramolecular hydrogen bonding
 and metal-binding ability.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12220
_journal_page_last               12227
_journal_paper_doi               10.1039/c3dt51389k
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C57 H66 Mn3 N4 O11, 0.5(C H2 Cl2), 1.5(C H4 O)'
_chemical_formula_sum            'C59 H73 Cl Mn3 N4 O12.5'
_chemical_formula_weight         1238.48
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      152
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   28.354(12)
_cell_length_b                   28.354(12)
_cell_length_c                   14.616(6)
_cell_measurement_reflns_used    24523
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      3.1361
_cell_volume                     10176(7)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -115.0000 - 65.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 54.8057
              2theta: -25.1617
scan:
    Number of images: 360
               Slice: -115.0000 - 65.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 54.8057
              2theta: -25.1617
scan:
    Number of images: 360
               Slice: -115.0000 - 65.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 54.8057
              2theta: -25.1617

;
_diffrn_measurement_device       'Saturn724+ (4x4 bin mode)'
_diffrn_measurement_device_details 'AFC11 (Right): Eulerian 3 circle'
_diffrn_measurement_device_type  'Rigaku AFC11 with Saturn 724+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            102462
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.14
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  0.9562
_exptl_absorpt_correction_T_min  0.7644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            'Dark Green'
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3882
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
The total void volume calculated by PLATON is 2417 A3 per unit cell (23.7%). 
The largest void (22.9%) is centered at the origin, which is filled with 
heavily disordered solvent molecules. The data were corrected with the SQUEEZE 
procedure implemented in PLATON to remove the contribution of the disordered 
solvent molecules to the structure factors. The SQUEEZE program suggested that 
the void space contains three dichloromethane and three methanol molecules 
per unit cell, which were removed from the model, but included in the formula.
;
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         15561
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0725
_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^)+(0.1046P)^2^+0.0897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1924
_refine_ls_wR_factor_ref         0.1992
_reflns_number_gt                13888
_reflns_number_total             15561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51389k.txt
_cod_data_source_block           Mn3-L-N2O2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        10177(7)
_cod_original_sg_symbol_H-M      P3121
_cod_original_formula_sum        'C59 H73 Cl Mn3 N4 O12.50'
_cod_database_code               7021794