#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:35:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179147 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/08/4310880.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4310880
loop_
_publ_author_name
'Avelino Martín'
'Miguel Mena'
'Adrián Pérez-Redondo'
'Carlos Yélamos'
_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       'κ-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/[σ²(Fo²)+(0.0236P)²+7.2060P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.8053(2) 0.8456(2) 0.3212(2) 0.0433(9) Uani 1 1 d . . .
C12 C 0.8020(2) 0.7948(2) 0.2540(2) 0.0421(9) Uani 1 1 d . . .
C13 C 0.7725(2) 0.8161(2) 0.1814(2) 0.0442(9) Uani 1 1 d . . .
C14 C 0.7576(2) 0.8803(2) 0.2043(2) 0.0463(9) Uani 1 1 d . . .
C15 C 0.7781(2) 0.8980(2) 0.2905(2) 0.0461(9) Uani 1 1 d . . .
C16 C 0.8341(4) 0.8436(5) 0.4104(3) 0.0731(16) Uani 1 1 d . . .
C17 C 0.8201(4) 0.7263(3) 0.2580(4) 0.0637(13) Uani 1 1 d . . .
C18 C 0.7598(4) 0.7766(4) 0.0956(4) 0.0750(16) Uani 1 1 d . . .
C19 C 0.7230(4) 0.9184(4) 0.1459(4) 0.0756(15) Uani 1 1 d . . .
C20 C 0.7669(4) 0.9588(4) 0.3432(4) 0.0740(16) Uani 1 1 d . . .
N1 N 1 1 0.2852(2) 0.0313(11) Uani 1 3 d S . .
N2 N 0.96866(19) 0.8956(2) 0.16067(18) 0.0360(7) Uani 1 1 d . . .
Rb1 Rb 1 1 0 0.0562(3) Uani 1 6 d S . .
Ti1 Ti 0.90316(3) 0.93254(3) 0.21912(3) 0.0319(2) Uani 1 1 d . . .
H2 H 0.960(3) 0.858(3) 0.147(3) 0.034(15) Uiso 0.83 1 d P . .
H16A H 0.877(4) 0.828(4) 0.406(4) 0.12(2) Uiso 1 1 d . . .
H16B H 0.797(4) 0.797(4) 0.439(4) 0.14(3) Uiso 1 1 d . . .
H16C H 0.817(4) 0.865(4) 0.432(4) 0.08(2) Uiso 1 1 d . . .
H17A H 0.842(3) 0.722(3) 0.299(3) 0.09(2) Uiso 1 1 d . . .
H17B H 0.773(3) 0.672(3) 0.257(3) 0.084(16) Uiso 1 1 d . . .
H17C H 0.857(3) 0.725(3) 0.224(3) 0.090(18) Uiso 1 1 d . . .
H18A H 0.787(3) 0.742(3) 0.087(3) 0.11(2) Uiso 1 1 d . . .
H18B H 0.702(4) 0.732(4) 0.086(4) 0.16(3) Uiso 1 1 d . . .
H18C H 0.764(4) 0.803(4) 0.059(4) 0.13(3) Uiso 1 1 d . . .
H19A H 0.670(5) 0.896(4) 0.148(4) 0.13(3) Uiso 1 1 d . . .
H19B H 0.746(5) 0.935(4) 0.085(6) 0.19(3) Uiso 1 1 d . . .
H19C H 0.723(3) 0.959(3) 0.173(3) 0.077(18) Uiso 1 1 d . . .
H20A H 0.758(3) 0.995(4) 0.309(4) 0.11(2) Uiso 1 1 d . . .
H20B H 0.810(3) 0.986(3) 0.381(4) 0.10(2) Uiso 1 1 d . . .
H20C H 0.724(4) 0.934(3) 0.376(4) 0.11(2) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 0 3
4 2 1
0 8 2
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 C11 C12 108.1(3) . . ?
C15 C11 C16 126.6(4) . . ?
C12 C11 C16 125.3(5) . . ?
C15 C11 Ti1 73.3(2) . . ?
C12 C11 Ti1 73.32(19) . . ?
C16 C11 Ti1 118.9(3) . . ?
C11 C12 C13 107.8(3) . . ?
C11 C12 C17 127.2(4) . . ?
C13 C12 C17 124.9(4) . . ?
C11 C12 Ti1 72.3(2) . . ?
C13 C12 Ti1 73.7(2) . . ?
C17 C12 Ti1 123.1(3) . . ?
C14 C13 C12 108.0(3) . . ?
C14 C13 C18 127.0(4) . . ?
C12 C13 C18 125.0(4) . . ?
C14 C13 Ti1 73.1(2) . . ?
C12 C13 Ti1 72.03(19) . . ?
C18 C13 Ti1 120.5(3) . . ?
C15 C14 C13 107.5(3) . . ?
C15 C14 C19 127.8(4) . . ?
C13 C14 C19 124.6(4) . . ?
C15 C14 Ti1 71.95(19) . . ?
C13 C14 Ti1 72.8(2) . . ?
C19 C14 Ti1 122.7(3) . . ?
C11 C15 C14 108.6(3) . . ?
C11 C15 C20 125.4(4) . . ?
C14 C15 C20 125.9(4) . . ?
C11 C15 Ti1 72.40(19) . . ?
C14 C15 Ti1 74.0(2) . . ?
C20 C15 Ti1 123.0(3) . . ?
Ti1 N1 Ti1 93.42(14) . 3_675 ?
Ti1 N1 Ti1 93.42(14) . 2_765 ?
Ti1 N1 Ti1 93.42(14) 3_675 2_765 ?
Ti1 N2 Ti1 93.66(15) 2_765 . ?
Ti1 N2 Rb1 96.94(12) 2_765 . ?
Ti1 N2 Rb1 96.74(12) . . ?
N2 Rb1 N2 180 2_765 11_565 ?
N2 Rb1 N2 58.82(11) 2_765 3_675 ?
N2 Rb1 N2 121.18(11) 11_565 3_675 ?
N2 Rb1 N2 121.18(11) 2_765 10_775 ?
N2 Rb1 N2 58.82(11) 11_565 10_775 ?
N2 Rb1 N2 121.18(11) 3_675 10_775 ?
N2 Rb1 N2 58.82(11) 2_765 . ?
N2 Rb1 N2 121.18(11) 11_565 . ?
N2 Rb1 N2 58.82(11) 3_675 . ?
N2 Rb1 N2 180 10_775 . ?
N2 Rb1 N2 121.18(11) 2_765 12_655 ?
N2 Rb1 N2 58.82(11) 11_565 12_655 ?
N2 Rb1 N2 180 3_675 12_655 ?
N2 Rb1 N2 58.82(11) 10_775 12_655 ?
N2 Rb1 N2 121.18(11) . 12_655 ?
N2 Rb1 Ti1 29.89(6) 2_765 3_675 ?
N2 Rb1 Ti1 150.11(6) 11_565 3_675 ?
N2 Rb1 Ti1 30.06(6) 3_675 3_675 ?
N2 Rb1 Ti1 120.38(7) 10_775 3_675 ?
N2 Rb1 Ti1 59.62(7) . 3_675 ?
N2 Rb1 Ti1 149.94(6) 12_655 3_675 ?
N2 Rb1 Ti1 150.11(6) 2_765 12_655 ?
N2 Rb1 Ti1 29.89(6) 11_565 12_655 ?
N2 Rb1 Ti1 149.94(6) 3_675 12_655 ?
N2 Rb1 Ti1 59.62(7) 10_775 12_655 ?
N2 Rb1 Ti1 120.38(7) . 12_655 ?
N2 Rb1 Ti1 30.06(6) 12_655 12_655 ?
Ti1 Rb1 Ti1 180 3_675 12_655 ?
N2 Rb1 Ti1 149.94(6) 2_765 11_565 ?
N2 Rb1 Ti1 30.06(6) 11_565 11_565 ?
N2 Rb1 Ti1 120.38(7) 3_675 11_565 ?
N2 Rb1 Ti1 29.89(6) 10_775 11_565 ?
N2 Rb1 Ti1 150.11(6) . 11_565 ?
N2 Rb1 Ti1 59.62(7) 12_655 11_565 ?
Ti1 Rb1 Ti1 136.93(3) 3_675 11_565 ?
Ti1 Rb1 Ti1 43.07(3) 12_655 11_565 ?
N2 Rb1 Ti1 30.06(6) 2_765 2_765 ?
N2 Rb1 Ti1 149.94(6) 11_565 2_765 ?
N2 Rb1 Ti1 59.62(7) 3_675 2_765 ?
N2 Rb1 Ti1 150.11(6) 10_775 2_765 ?
N2 Rb1 Ti1 29.89(6) . 2_765 ?
N2 Rb1 Ti1 120.38(7) 12_655 2_765 ?
Ti1 Rb1 Ti1 43.07(3) 3_675 2_765 ?
Ti1 Rb1 Ti1 136.93(3) 12_655 2_765 ?
Ti1 Rb1 Ti1 180.000(19) 11_565 2_765 ?
N2 Rb1 Ti1 59.62(7) 2_765 . ?
N2 Rb1 Ti1 120.38(7) 11_565 . ?
N2 Rb1 Ti1 29.89(6) 3_675 . ?
N2 Rb1 Ti1 149.94(6) 10_775 . ?
N2 Rb1 Ti1 30.06(6) . . ?
N2 Rb1 Ti1 150.11(6) 12_655 . ?
Ti1 Rb1 Ti1 43.07(3) 3_675 . ?
Ti1 Rb1 Ti1 136.93(3) 12_655 . ?
Ti1 Rb1 Ti1 136.93(3) 11_565 . ?
Ti1 Rb1 Ti1 43.07(3) 2_765 . ?
N2 Rb1 Ti1 120.38(7) 2_765 10_775 ?
N2 Rb1 Ti1 59.62(7) 11_565 10_775 ?
N2 Rb1 Ti1 150.11(6) 3_675 10_775 ?
N2 Rb1 Ti1 30.06(6) 10_775 10_775 ?
N2 Rb1 Ti1 149.94(6) . 10_775 ?
N2 Rb1 Ti1 29.89(6) 12_655 10_775 ?
Ti1 Rb1 Ti1 136.93(3) 3_675 10_775 ?
Ti1 Rb1 Ti1 43.07(3) 12_655 10_775 ?
Ti1 Rb1 Ti1 43.07(3) 11_565 10_775 ?
Ti1 Rb1 Ti1 136.93(3) 2_765 10_775 ?
Ti1 Rb1 Ti1 180.00(2) . 10_775 ?
N2 Ti1 N1 86.35(12) 3_675 . ?
N2 Ti1 N2 103.77(19) 3_675 . ?
N1 Ti1 N2 86.10(12) . . ?
N2 Ti1 C11 135.93(14) 3_675 . ?
N1 Ti1 C11 103.83(14) . . ?
N2 Ti1 C11 119.44(14) . . ?
N2 Ti1 C15 102.20(14) 3_675 . ?
N1 Ti1 C15 113.76(13) . . ?
N2 Ti1 C15 148.14(14) . . ?
C11 Ti1 C15 34.30(13) . . ?
N2 Ti1 C12 146.71(14) 3_675 . ?
N1 Ti1 C12 124.63(12) . . ?
N2 Ti1 C12 91.43(13) . . ?
C11 Ti1 C12 34.37(12) . . ?
C15 Ti1 C12 56.93(13) . . ?
N2 Ti1 C13 113.56(13) 3_675 . ?
N1 Ti1 C13 158.73(12) . . ?
N2 Ti1 C13 95.75(14) . . ?
C11 Ti1 C13 56.94(12) . . ?
C15 Ti1 C13 56.66(13) . . ?
C12 Ti1 C13 34.32(12) . . ?
N2 Ti1 C14 90.88(14) 3_675 . ?
N1 Ti1 C14 145.88(12) . . ?
N2 Ti1 C14 127.38(14) . . ?
C11 Ti1 C14 56.95(13) . . ?
C15 Ti1 C14 34.09(13) . . ?
C12 Ti1 C14 56.97(13) . . ?
C13 Ti1 C14 34.12(13) . . ?
N2 Ti1 Ti1 43.30(10) 3_675 3_675 ?
N1 Ti1 Ti1 43.29(7) . 3_675 ?
N2 Ti1 Ti1 93.19(10) . 3_675 ?
C11 Ti1 Ti1 134.18(9) . 3_675 ?
C15 Ti1 Ti1 118.45(10) . 3_675 ?
C12 Ti1 Ti1 166.53(8) . 3_675 ?
C13 Ti1 Ti1 156.77(9) . 3_675 ?
C14 Ti1 Ti1 127.74(9) . 3_675 ?
N2 Ti1 Ti1 93.39(10) 3_675 2_765 ?
N1 Ti1 Ti1 43.29(7) . 2_765 ?
N2 Ti1 Ti1 43.05(10) . 2_765 ?
C11 Ti1 Ti1 123.50(10) . 2_765 ?
C15 Ti1 Ti1 151.73(10) . 2_765 ?
C12 Ti1 Ti1 117.10(10) . 2_765 ?
C13 Ti1 Ti1 136.55(10) . 2_765 ?
C14 Ti1 Ti1 170.31(10) . 2_765 ?
Ti1 Ti1 Ti1 60 3_675 2_765 ?
N2 Ti1 Rb1 53.17(9) 3_675 . ?
N1 Ti1 Rb1 97.73(10) . . ?
N2 Ti1 Rb1 53.20(9) . . ?
C11 Ti1 Rb1 156.82(9) . . ?
C15 Ti1 Rb1 139.42(10) . . ?
C12 Ti1 Rb1 123.91(8) . . ?
C13 Ti1 Rb1 100.31(9) . . ?
C14 Ti1 Rb1 107.65(9) . . ?
Ti1 Ti1 Rb1 68.467(13) 3_675 . ?
Ti1 Ti1 Rb1 68.467(13) 2_765 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 C15 1.401(5) . ?
C11 C12 1.405(5) . ?
C11 C16 1.513(6) . ?
C11 Ti1 2.371(3) . ?
C12 C13 1.413(5) . ?
C12 C17 1.485(6) . ?
C12 Ti1 2.384(3) . ?
C13 C14 1.412(5) . ?
C13 C18 1.502(6) . ?
C13 Ti1 2.405(3) . ?
C14 C15 1.404(5) . ?
C14 C19 1.498(6) . ?
C14 Ti1 2.408(3) . ?
C15 C20 1.506(6) . ?
C15 Ti1 2.382(3) . ?
N1 Ti1 1.920(2) . ?
N1 Ti1 1.920(2) 3_675 ?
N1 Ti1 1.920(2) 2_765 ?
N2 Ti1 1.912(3) 2_765 ?
N2 Ti1 1.921(3) . ?
N2 Rb1 3.070(3) . ?
Rb1 N2 3.070(3) 2_765 ?
Rb1 N2 3.070(3) 11_565 ?
Rb1 N2 3.070(3) 3_675 ?
Rb1 N2 3.070(3) 10_775 ?
Rb1 N2 3.070(3) 12_655 ?
Rb1 Ti1 3.8082(17) 3_675 ?
Rb1 Ti1 3.8082(17) 12_655 ?
Rb1 Ti1 3.8082(17) 11_565 ?
Rb1 Ti1 3.8082(17) 2_765 ?
Rb1 Ti1 3.8082(17) . ?
Rb1 Ti1 3.8082(17) 10_775 ?
Ti1 N2 1.912(3) 3_675 ?
Ti1 Ti1 2.7954(13) 3_675 ?
Ti1 Ti1 2.7954(13) 2_765 ?
