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_7021793
_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_formula_moiety
'C55 H68 Mn2 N4 O9, 0.5(C H2 Cl2), 2.5(C H4 O), 0.5(H2 O)'
_chemical_formula_sum            'C58 H80 Cl Mn2 N4 O12'
_chemical_formula_weight         1170.59
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 92.290(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.540(7)
_cell_length_b                   12.330(3)
_cell_length_c                   25.680(6)
_cell_measurement_reflns_used    13877
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4831
_cell_measurement_theta_min      4.0032
_cell_volume                     11561(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
scan:
    Number of images: 600
               Slice: -80.0000 - 100.000
         Image width: 0.3000
            Exp time: 10.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 45.2335
              2theta: 19.7960
scan:
    Number of images: 160
               Slice: -20.0000 - 28.0000
         Image width: 0.3000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 45.2335
              2theta: 19.7960
scan:
    Number of images: 160
               Slice: -20.0000 - 28.0000
         Image width: 0.3000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 45.2335
              2theta: 19.7960
scan:
    Number of images: 160
               Slice: -20.0000 - 28.0000
         Image width: 0.3000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 45.2335
              2theta: 19.7960
scan:
    Number of images: 160
               Slice: -20.0000 - 28.0000
         Image width: 0.3000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 270.0000
                 XTD: 45.2335
              2theta: 19.7960

;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details 'AFC7: Eulerian 3-circle'
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\w or \f'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44290
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.01
_diffrn_source_current           200.0000
_diffrn_source_power             11.0000
_diffrn_source_voltage           55.0000
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.9838
_exptl_absorpt_correction_T_min  0.7909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4952
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 150(2) K'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     744
_refine_ls_number_reflns         12938
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.230
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0835
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+48.6150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1579
_reflns_number_gt                11324
_reflns_number_total             12938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51389k.txt
_cod_data_source_block           Mn2-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_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7021793