Syntheses, solid state and solution structures of [Ba{(C~5~Me~5~)~2~Ti~2~F~7~}~2~(HMPA)] and [Ba~8~Ti~6~F~30~I~2~(C~5~Me~5~)~6~(HMPA)~6~][I~3~]~2~
Andrej Pevec; Inorganic Chemistry 43 (2004) 1250–1256; doi:10.1021/ic035256v

data_4310635
_publ_contact_author_address
;
Faculty of Chemistry and Chemical Technology
University of Ljubljana
A\<sker\<ceva 5, P. O. Box 537
1000 Ljubljana
Slovenia
;
_publ_contact_author_email       andrej.pevec@uni-lj.si
_publ_contact_author_name        'Andrej Pevec'
_publ_section_title
;
 Syntheses, solid state and solution structures of
 [Ba{(C~5~Me~5~)~2~Ti~2~F~7~}~2~(HMPA)] and
 [Ba~8~Ti~6~F~30~I~2~(C~5~Me~5~)~6~(HMPA)~6~][I~3~]~2~
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1250
_journal_page_last               1256
_journal_paper_doi               10.1021/ic035256v
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C136 H278 Ba8 F30 I8 N18 O16 P6 Ti6'
_chemical_formula_weight         5578.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.7230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   41.1535(5)
_cell_length_b                   16.7918(2)
_cell_length_c                   33.7062(4)
_cell_measurement_reflns_used    13279
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     21925.9(5)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Reference Manual (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.390
_diffrn_measured_fraction_theta_max 0.390
_diffrn_measurement_device_type
;
Nonius KappaCCD area-detector diffractometer (with an Oxford Cryostream cooler)
;
_diffrn_measurement_method       '\w scans at fixed \c = 55\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0642
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            29651
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    2.861
_exptl_absorpt_correction_T_max  0.7629
_exptl_absorpt_correction_T_min  0.5591
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             10848
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.715
_refine_diff_density_min         -3.876
_refine_diff_density_rms         0.341
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     971
_refine_ls_number_reflns         20244
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0761
_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^)+(0.1189P)^2^+704.6227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2039
_refine_ls_wR_factor_ref         0.2471
_reflns_number_gt                14247
_reflns_number_total             20244
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035256vsi20031030_081750_1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1189P)^2^+704.6227P] 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^)+(0.1189P)^2^+704.6227P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4310635