Low-Temperature Structures of <i>fac</i>-Trichloro(tetrahydrofuran)(<small>D</small>, <small>L</small>-tetrahydrofurfuranol)titanium(III) and <i>fac</i>-Trichloro(tetrahydrofuran)(<small>D</small>, <small>L</small>-tetrahydrofurfuroxide)titanium(IV)
Olejnik, Z.; Lis, T.; Utko, J.; Sobota, P.; Acta Crystallographica Section C 52 (1996) 847–850; doi:10.1107/S0108270195013485

data_2004754
_publ_section_title
;
 Low-Temperature Structures of
 <i>fac</i>-Trichloro(tetrahydrofuran)(<small>D</small>,
 <small>L</small>-tetrahydrofurfuranol)titanium(III) and
 <i>fac</i>-Trichloro(tetrahydrofuran)(<small>D</small>,
 <small>L</small>-tetrahydrofurfuroxide)titanium(IV)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              847
_journal_page_last               850
_journal_paper_doi               10.1107/S0108270195013485
_journal_volume                  52
_journal_year                    1996
_chemical_formula_sum            'C9 H17 Cl3 O3 Ti'
_chemical_formula_weight         327.48
_chemical_name_systematic
;
fac-trichloro(tetrahydrofuran)(d,l-tetrahydrofurfuroxide)titanium(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.
_cell_angle_beta                 131.06(12)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   9.074(8)
_cell_length_b                   12.553(9)
_cell_length_c                   15.65(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      8.5
_cell_volume                     1344(3)
_computing_data_collection       'KM4 Software (Kuma Diffraction, 1989)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      80(2)
_diffrn_measurement_device
'Kuma KM4 computer-controlled four-circle \w/2\q diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3747
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_min         2
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.222
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green-yellow
_exptl_crystal_density_diffrn    1.618(5)
_exptl_crystal_density_meas      1.562
_exptl_crystal_density_method    'flotation in CCl~4~/CH~2~Cl~2~'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.107
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3233
_refine_ls_number_restraints     6
_refine_ls_R_factor_obs          0.0233
_refine_ls_shift/esd_max         0.172
_refine_ls_shift/esd_mean        0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.6656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0629
_reflns_number_observed          2955
_reflns_number_total             3233
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            jz1073.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.6656P] 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^)+(0.0348P)^2^+0.6656P] 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 21/c'
_cod_database_code               2004754