A novel titanium‒oxygen ladder structure supported by calix[4]arene ligands, characterised by synchrotron crystallography
Clegg, William; Elsegood, Mark R. J.; Teat, Simon J.; Redshaw, Carl; Gibson, Vernon C.; Journal of the Chemical Society, Dalton Transactions  (1998) 3037–; doi:10.1039/a803864c

data_7027975
_publ_section_title
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 A novel titanium--oxygen ladder structure supported by calix[4]arene
 ligands, characterised by synchrotron crystallography
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3037
_journal_paper_doi               10.1039/a803864c
_journal_year                    1998
_chemical_formula_sum            'C102 H120 Cl4 O10 Ti4'
_chemical_formula_weight         1839.38
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.299(3)
_cell_angle_beta                 68.935(3)
_cell_angle_gamma                85.043(3)
_cell_formula_units_Z            1
_cell_length_a                   12.5692(14)
_cell_length_b                   13.4268(15)
_cell_length_c                   15.4275(17)
_cell_measurement_reflns_used    8219
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      1.69
_cell_volume                     2420.0(5)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6879
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.1058
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11915
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.281
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.0040(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         9287
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1498
_reflns_number_gt                6241
_reflns_number_total             9287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c803864sup1.cif
_cod_data_source_block           vcg129
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027975