Molecular Recognition of Titanium(IV) Alkoxides by 2,6-Bis(hydroxymethyl)-p-cresol in the Crystal Engineering of Hybrid Organic-Inorganic Networks
Adel Rammal; Frédéric Brisach; Marc Henry; Journal of the American Chemical Society 123 (2001) 5612–5613; doi:10.1021/ja0156136

data_4115568
_publ_contact_author_address
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Universit\'e Louis Pasteur, Institut Le Bel
Laboratoire de Chimie Mol\'eculaire de l'\'Etat Solide
UMR CNRS/ULP 7513
4, Rue Blaise Pascal
67070 Strasbourg Cedex, France
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_publ_contact_author_email       henry@chimie.u-strasbg.fr
_publ_contact_author_fax         +33.3.88.41.53.13
_publ_contact_author_name        'Marc HENRY'
_publ_contact_author_phone       +33.3.88.41.53.13
_publ_section_title
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 Molecular Recognition of Titanium(IV) Alkoxides by
 2,6-Bis(hydroxymethyl)-p-cresol in the Crystal Engineering of Hybrid
 Organic-Inorganic Networks
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5612
_journal_page_last               5613
_journal_paper_doi               10.1021/ja0156136
_journal_volume                  123
_journal_year                    2001
_chemical_compound_source        Synthetic
_chemical_formula_moiety         'C131 H162 Cl18 O49 Ti8'
_chemical_formula_structural
{[Ti4O2(BHMPC)6][1,4-dioxanne]2[CHCl3]2.CHCl3}2.(CO)
_chemical_formula_sum            'C131 H162 Cl18 O49 Ti8'
_chemical_formula_weight         3542.08
_chemical_name_common            Ti4_BHMPC_CHCL3
_chemical_name_systematic        ' ?'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                81.271(6)
_cell_angle_beta                 77.401(6)
_cell_angle_gamma                81.550(6)
_cell_formula_units_Z            1
_cell_length_a                   12.8922(4)
_cell_length_b                   14.1422(4)
_cell_length_c                   22.8758(4)
_cell_measurement_reflns_used    18102
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     3995.1(2)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
  18102 reflections were collected using program Collect
 ("Collect" Data collection software, Nonius B.V., 1998)
 The conditions were as follow : crystal to detector distance =  36. mm.
 Scan angle =  1.5 deg 1 scans of   90 sec per frame.
 Data collection was divided into  3 set(s)
 with the following starting angles and number of frames :

 Set 1 Theta =    6.40 Omega =    0.00 Kappa =    0.00  122 frames
 Set 2 Theta =   -3.70 Kappa = -174.00 Phi   =    0.00   30 frames
 Set 3 Theta =   -3.80 Kappa =  139.00 Phi   =    0.00   17 frames
 Friedel pairs were averaged. Internal R = 0.05
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            18102
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.47
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1822
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.244
_refine_diff_density_min         -0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   5.682
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     897
_refine_ls_number_reflns         10414
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.164
_refine_ls_R_factor_gt           0.099
_refine_ls_shift/esd_mean        0.002
_refine_ls_shift/su_max          0.077
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0004 Fo^4^)+0.6'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.429
_refine_ls_wR_factor_ref         0.122
_reflns_number_gt                10414
_reflns_number_total             18102
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            ja0156136_s2_2.cif
_cod_data_source_block           st592
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^)+0.0004
Fo^4^)+0.6' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0004 Fo^4^)+0.6'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        3995.1(1)
_cod_database_code               4115568