Cube-Type Nitrido Complexes Containing Titanium and Alkali/Alkaline-Earth Metals
Avelino Martín; Miguel Mena; Adrián Pérez-Redondo; Carlos Yélamos; Inorganic Chemistry 43 (2004) 2491–2498; doi:10.1021/ic035493y

data_4310880
_publ_section_title
;
 Cube-Type Nitrido Complexes Containing Titanium and Alkali/Alkaline-Earth
 Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2491
_journal_page_last               2498
_journal_paper_doi               10.1021/ic035493y
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C60 H95 N8 Rb1 Ti6'
_chemical_formula_structural     'RB1 TI6 N8 C60 H95'
_chemical_formula_sum            'C60 H95 N8 Rb Ti6'
_chemical_formula_weight         1301.31
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2001-10-26T12:00:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.767(6)
_cell_length_b                   18.767(6)
_cell_length_c                   15.741(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      6
_cell_measurement_wavelength     0.71073
_cell_volume                     4801(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.28547E-1
_diffrn_orient_matrix_UB_12      0.39382E-1
_diffrn_orient_matrix_UB_13      0.32305E-1
_diffrn_orient_matrix_UB_21      -0.00638
_diffrn_orient_matrix_UB_22      -0.32894E-1
_diffrn_orient_matrix_UB_23      0.62189E-1
_diffrn_orient_matrix_UB_31      0.64177E-1
_diffrn_orient_matrix_UB_32      0.14179E-1
_diffrn_orient_matrix_UB_33      0.54053E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1061
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4665
_diffrn_reflns_theta_full        22.99
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         1.8
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        13
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.51
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.35
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         1493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+7.2060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                1250
_reflns_number_total             1493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035493ysi20031230_055534_2.cif
_cod_data_source_block           9
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4310880