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_4115567
_publ_contact_author_address
;
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
;
_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
;
 Molecular Recognition of Titanium(IV) Alkoxides by
 2,6-Bis(hydroxymethyl)-p-cresol in the Crystal Engineering of Hybrid
 Organic-Inorganic Networks
;
_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         'C66 H86 O26 Ti4'
_chemical_formula_structural     '[Ti4O2(BHMPC)6][1,4-dioxanne]2[EtOH]2'
_chemical_formula_sum            'C66 H86 O26 Ti4'
_chemical_formula_weight         1487.01
_chemical_name_common            Ti4_BHMPC_ETOH
_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                80.769(5)
_cell_angle_beta                 70.036(5)
_cell_angle_gamma                77.303(5)
_cell_formula_units_Z            1
_cell_length_a                   11.1076(9)
_cell_length_b                   11.871(2)
_cell_length_c                   14.655(2)
_cell_measurement_reflns_used    9021
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     1764.2(4)
_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
;
    9021 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   20 sec per frame.
  Data collection was divided into  1 set(s)
  with the following starting angles and number of frames :

  Set 1 Theta =    6.30 Omega =    0.00 Kappa =    0.00   91 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       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9021
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.40
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   6.920
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     388
_refine_ls_number_reflns         3131
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.193
_refine_ls_R_factor_gt           0.082
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.009
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.515
_refine_ls_wR_factor_ref         0.104
_reflns_number_gt                3131
_reflns_number_total             6944
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            ja0156136_s2_1.cif
_cod_data_source_block           st657
_cod_original_cell_volume        1764.1(5)
_cod_database_code               4115567