A new double-cube nitride complex containing titanium and potassium
Martín, Avelino; Mena, Miguel; Pérez-Redondo, Adrián; Yélamos, Carlos; Acta Crystallographica Section C 67 (2011) m157–m159; doi:10.1107/S0108270111012686

data_2018057
_publ_section_title
;
 A new double-cube nitride complex containing titanium and potassium
;
_journal_coeditor_code           DT3001
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m157
_journal_page_last               m159
_journal_paper_doi               10.1107/S0108270111012686
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[K2 Ti6 (C10 H15)6 I2 N2 (N H)6 (C5 H5 N)2]'
_chemical_formula_moiety         'C70 H106 I2 K2 N10 Ti6'
_chemical_formula_sum            'C70 H106 I2 K2 N10 Ti6'
_chemical_formula_weight         1707.05
_chemical_name_systematic
;
di-\m-iodido-1:1'\k^4^<i>I</i>-bis[tri-\m~3~-imido-1:2:3\k^3^<i>N</i>;
1:2:4\k^3^<i>N</i>;1:3:4\k^3^<i>N</i>-\m~3~-nitrido-2:3:4\k^3^<i>N</i>-
tris[2,3,4(\h^5^)-pentamethylcyclopentadienyl](pyridine-1\k<i>N</i>)-
<i>tetrahedro</i>-potassiumtrititanium(IV)]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                101.660(10)
_cell_angle_beta                 93.460(10)
_cell_angle_gamma                115.550(10)
_cell_formula_units_Z            1
_cell_length_a                   11.298(2)
_cell_length_b                   11.346(2)
_cell_length_c                   18.391(3)
_cell_measurement_reflns_used    82
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      3
_cell_volume                     2053.8(7)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'EVALCCD (Duisenberg <i>et al.</i>, 2003)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34701
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R. H. Blessing (1987), Cryst. Rev. 1, 3--58
 R. H. Blessing (1989), J. Appl. Cryst. 22, 396--397
;
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    1.45
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.38
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.82
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         9150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.047
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0609P)^2^+0.0977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1192
_reflns_number_gt                6034
_reflns_number_total             9150
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dt3001.cif
_cod_data_source_block           II
_cod_original_cell_volume        2053.8(6)
_cod_database_code               2018057
_cod_database_fobs_code          2018057