Tetrabromo(2-methylpyridine-<i>N</i>)titanate(IV)
Hensen, Karl; Lemke, Alexander; Bolte, Michael; Acta Crystallographica Section C 56 (2000) e565–e566; doi:10.1107/S0108270100015407

data_2011652
_publ_section_title
;
 Tetrabromo(2-methylpyridine-<i>N</i>)titanate(IV)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e565
_journal_page_last               e566
_journal_paper_doi               10.1107/S0108270100015407
_journal_volume                  56
_journal_year                    2000
_chemical_formula_sum            'C6 H7 Br4 N Ti'
_chemical_formula_weight         460.67
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 91.8200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.74160(10)
_cell_length_b                   9.8984(2)
_cell_length_c                   17.3338(3)
_cell_measurement_reflns_used    6306
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.00
_cell_volume                     1156.12(4)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full .874
_diffrn_measured_fraction_theta_max .874
_diffrn_measurement_device       'Siemens CCD three-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'highly oriented graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .086
_diffrn_reflns_av_sigmaI/netI    .0706
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15542
_diffrn_reflns_theta_full        26.21
_diffrn_reflns_theta_max         26.21
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  1000
_diffrn_standards_number         131
_exptl_absorpt_coefficient_mu    14.515
_exptl_absorpt_correction_T_max  .055
_exptl_absorpt_correction_T_min  .026
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
The data collection nominally covered a sphere of reciprocal
space, by a combination of seven sets of exposures; each set had a
different \f angle for the crystal and each exposure covered 0.3\% in \w.
The crystal-to-detector distance was 6 cm.
Coverage of the unique set for all structures
is 100% complete to at least 25.0\% in \q. Crystal decay was
monitored by repeating the initial frames at the end of data collection and
analyzing the duplicate reflections.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .20
_refine_diff_density_max         .976
_refine_diff_density_min         -.924
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.088
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          .093
_refine_ls_R_factor_obs          .055
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0402P)^2^+4.5123P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .106
_refine_ls_wR_factor_obs         .095
_refine_ls_wR_factor_ref         .106
_reflns_number_gt                1587
_reflns_number_total             2159
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qa0449.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0402P)^2^+4.5123P] 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^)+(0.0402P)^2^+4.5123P] 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/n'
_cod_database_code               2011652
_cod_database_fobs_code          2011652