A novel titanium‒μ-O‒zirconium complex: bis(μ-methyliminodiethanolato-1κ^3^<i>O</i>,<i>N</i>,<i>O</i>';1:2κ^2^<i>O</i>)(methyliminodiethanolato-2κ^3^<i>O</i>,<i>N</i>,<i>O</i>')dipropanolato-1κ<i>O</i>,2κ<i>O</i>-titanium(IV)zirconium(IV)
Gainsford, Graeme J.; Al-Salim, Najeh; Kemmitt, Tim; Acta Crystallographica Section C 58 (2002) m509–m510; doi:10.1107/S0108270102015275

data_2013003
_publ_section_title
;A novel titanium--\m-O--zirconium complex:
 bis(\m-methyliminodiethanolato-1\k^3^<i>O</i>,<i>N</i>,<i>O</i>';1:2\k^2^<i>O</i>)(methyliminodiethanolato-2\k^3^<i>O</i>,<i>N</i>,<i>O</i>')dipropanolato-1\k<i>O</i>,2\k<i>O</i>-titanium(IV)zirconium(IV)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m509
_journal_page_last               m510
_journal_paper_doi               10.1107/S0108270102015275
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Ti Zr (C5 H11 N O2)3 (C3 H7 O)2]'
_chemical_formula_moiety         'C21 H47 N3 O8 Ti Zr'
_chemical_formula_structural
'Zr (C5 H11 N O2)2 (C3 H7 O) Ti (C5 H11 N O2) (C3 H7 O)'
_chemical_formula_sum            'C21 H47 N3 O8 Ti Zr'
_chemical_formula_weight         608.74
_chemical_name_systematic
;bis(\m-methyliminodiethanolato-1\k^3^O,N,O';1:2\k^2^O)(methyliminodiethanolato-
2\k^3^O,N,O')dipropanolato-1\kO,2\kO-titanium(IV)zirconium(IV)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 116.002(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.172(10)
_cell_length_b                   10.407(3)
_cell_length_c                   19.116(6)
_cell_measurement_reflns_used    5093
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      2.6
_cell_volume                     5574(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction
'SAINT (Siemens, 1996) and SADABS (Sheldrick, 1996)'
_computing_molecular_graphics    'ORTEP-3 in WinGX (Farrugia, 1997, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      163(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Make Model CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.056
_diffrn_reflns_av_sigmaI/netI    0.075
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            19935
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.71
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cubic block'
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.59
_refine_ls_extinction_coef       0.00051(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   0.95
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5613
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.95
_refine_ls_R_factor_all          0.072
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0537P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.098
_refine_ls_wR_factor_ref         0.104
_reflns_number_gt                3723
_reflns_number_total             5613
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ta1389.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (13 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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 2.4.1 from 2010-06-29.

'_geom_bond_publ_flag'
value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (13
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10
times).

'_geom_torsion_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (2 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 
;
_cod_original_cell_volume        5574(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2013003
_cod_database_fobs_code          2013003