#------------------------------------------------------------------------------
#$Date: 2019-11-17 06:11:49 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228340 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/20/7122025.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_7122025
loop_
_publ_author_name
'Goodwin, Conrad A. P.'
'Reta, Daniel'
'Ortu, Fabrizio'
'Liu, Jingjing'
'Chilton, Nicholas F.'
'Mills, David P.'
_publ_section_title
;
 Terbocenium: completing a heavy lanthanide metallocenium cation family
 with an alternative anion abstraction strategy.
;
_journal_issue                   66
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9182
_journal_page_last               9185
_journal_paper_doi               10.1039/c8cc05261a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C12 H34.54 B2.64 I0.36 O3 Tb'
_chemical_formula_sum            'C12 H34.54 B2.63 I0.37 O3 Tb'
_chemical_formula_weight         460.66
_chemical_name_systematic        '[Tb(BH4)3(THF)3]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-21 deposited with the CCDC.
2018-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1844(2)
_cell_length_b                   14.3006(3)
_cell_length_c                   14.7076(4)
_cell_measurement_reflns_used    8710
_cell_measurement_temperature    149.95(10)
_cell_measurement_theta_max      29.8080
_cell_measurement_theta_min      2.1950
_cell_volume                     1931.73(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -6.00  21.00   0.50    2.00    --   -7.80  21.00 -15.00   54
  2  ω    -43.00 -18.00   0.50    2.00    --   -7.80 -21.00 178.00   50
  3  ω    -94.00  31.00   0.50    2.00    --   -7.80 -38.00  30.00  250
  4  ω    -39.00  58.00   0.50    2.00    --   -7.80  57.00-150.00  194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0273237000
_diffrn_orient_matrix_UB_12      0.0026061000
_diffrn_orient_matrix_UB_13      -0.0450381000
_diffrn_orient_matrix_UB_21      -0.0691189000
_diffrn_orient_matrix_UB_22      0.0134569000
_diffrn_orient_matrix_UB_23      0.0170663000
_diffrn_orient_matrix_UB_31      0.0210514000
_diffrn_orient_matrix_UB_32      0.0476628000
_diffrn_orient_matrix_UB_33      -0.0023407000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12868
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.849
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.244
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.493
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.242
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1762
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.307
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+6.1771P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1731
_reflns_number_total             1762
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc05261a2.cif
_cod_data_source_block           1-Tb
_cod_depositor_comments
'Adding full bibliography for 7122025--7122029.cif.'
_cod_original_cell_volume        1931.72(8)
_cod_database_code               7122025
_manchester_internal_coll_name   rdpm80
_manchester_internal_coll_client CAPG/FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 2s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   18/11/17
_manchester_internal_process_user CAPG/FO
_manchester_internal_process_date 20/11/17
_manchester_internal_solution_user CAPG/FO
_manchester_internal_solution_date 20/11/17
_manchester_internal_refinement_user CAPG/FO
_manchester_internal_refinement_date 20/11/17
_manchester_internal_validation_user FO
_manchester_internal_validation_date 20/11/17
_manchester_internal_archive_date 20/11/17
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     FO/CAPG
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All I(H) groups
2. Restrained distances
 B2-H2A = B2-H2B
 1.1 with sigma of 0.02
 B1-H1D = B1-H1A = B1-H1B = B1-H1C
 1.1 with sigma of 0.02
 H1D-H1A
 1.5 with sigma of 0.02
 H1D-H1C
 1.5 with sigma of 0.02
 H1A-H1B
 1.5 with sigma of 0.02
 H1D-H1B
 1.5 with sigma of 0.02
 Tb1-B1 \\sim Tb1-B2
 with sigma of 0.02
 Tb1-H1B \\sim Tb1-H1A \\sim Tb1-H1D
 with sigma of 0.02
 H1C-H1A \\sim H1C-H1B \\sim H1C-H1D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B1 \\sim I2A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(I2A)=1-FVAR(1)
 Sof(H1A)=Sof(H1B)=Sof(H1D)=Sof(B1)=Sof(H1C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1E,H1F), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
;
_olex2_exptl_crystal_mounting_method 'in fomblin oil on micromount'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.132
_oxdiff_exptl_absorpt_empirical_full_min 0.646
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.500000 0.15286(2) 0.750000 0.02606(10) Uani 1 2 d DS TU P . .
H1A H 0.405(3) 0.176(3) 0.6016(17) 0.059(19) Uiso 0.8179(16) 1 d D . . A 1
H1B H 0.320(4) 0.0959(15) 0.648(3) 0.07(2) Uiso 0.8179(16) 1 d D . . A 1
H1D H 0.285(3) 0.197(3) 0.671(2) 0.07(2) Uiso 0.8179(16) 1 d D . . A 1
O1 O 0.6918(3) 0.11988(18) 0.64833(17) 0.0299(6) Uani 1 1 d . U . . .
O2 O 0.500000 -0.0174(2) 0.750000 0.0351(9) Uani 1 2 d S TU P A .
C1 C 0.7105(5) 0.1570(4) 0.5560(3) 0.0458(12) Uani 1 1 d . U . . .
H1E H 0.703374 0.224711 0.556230 0.055 Uiso 1 1 calc R . . . .
H1F H 0.636392 0.132170 0.515722 0.055 Uiso 1 1 calc R . . . .
C2 C 0.8593(5) 0.1267(4) 0.5257(3) 0.0490(12) Uani 1 1 d . U . . .
H2C H 0.859073 0.110137 0.461717 0.059 Uiso 1 1 calc R . . . .
H2D H 0.930261 0.175822 0.535668 0.059 Uiso 1 1 calc R . . . .
C3 C 0.8920(6) 0.0431(4) 0.5836(3) 0.0524(13) Uani 1 1 d . U . . .
H3A H 0.852487 -0.013425 0.556700 0.063 Uiso 1 1 calc R . . . .
H3B H 0.996175 0.035409 0.591646 0.063 Uiso 1 1 calc R . . . .
C4 C 0.8201(5) 0.0642(3) 0.6710(3) 0.0437(11) Uani 1 1 d . U . . .
H4A H 0.791929 0.006908 0.701657 0.052 Uiso 1 1 calc R . . . .
H4B H 0.884972 0.099112 0.710455 0.052 Uiso 1 1 calc R . . . .
C5 C 0.5178(6) -0.0774(3) 0.8293(3) 0.0514(12) Uani 1 1 d . U . . .
H5A H 0.455217 -0.056898 0.878525 0.062 Uiso 1 1 calc R . . A .
H5B H 0.617970 -0.076582 0.850179 0.062 Uiso 1 1 calc R . . . .
C6 C 0.4758(7) -0.1731(3) 0.7982(4) 0.0683(17) Uani 1 1 d . U . . .
H6A H 0.525729 -0.220985 0.833017 0.082 Uiso 1 1 calc R . . . .
H6B H 0.371571 -0.182752 0.802877 0.082 Uiso 1 1 calc R . . . .
B2 B 0.500000 0.3440(4) 0.750000 0.0320(13) Uani 1 2 d DS TU P A .
H2B H 0.567(6) 0.392(3) 0.788(4) 0.10(2) Uiso 1 1 d D . . . .
B1 B 0.302(2) 0.1566(10) 0.6157(11) 0.036(4) Uani 0.8179(16) 1 d D U . A 1
H1C H 0.225(3) 0.163(2) 0.571(2) 0.08(2) Uiso 0.8179(16) 1 d D . . A 1
I2A I 0.3051(5) 0.1324(3) 0.5984(3) 0.0401(10) Uani 0.1821(16) 1 d . U . A 2
H2A H 0.440(5) 0.298(3) 0.794(3) 0.060 Uiso 1 1 d DR . . . .
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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
12 -8 0 0.1820
-7 -16 1 0.1753
5 -18 1 0.1673
-2 20 -1 0.1735
-13 5 0 0.2017
11 2 -10 0.1237
10 -6 -10 0.1136
-11 5 11 0.1458
-6 -17 4 0.1681
4 13 15 0.1912
-1 4 -20 0.2021
3 19 -7 0.1481
4 19 1 0.1537
-3 -19 4 0.1382
-6 -11 -14 0.1985
-8 10 -13 0.2296
-11 10 -2 0.2065
-9 10 12 0.1310
-10 2 12 0.1489
-3 5 20 0.1215
5 -14 13 0.1760
9 10 11 0.2171
8 -6 15 0.2104
8 14 8 0.2013
9 3 -15 0.1053
8 -5 -15 0.0991
5 -14 -12 0.1523
6 6 -18 0.1280
4 -6 -19 0.1255
-5 9 17 0.1202
1 -4 20 0.1603
3 12 16 0.1847
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
O1 Tb1 O1 156.93(13) 4_656 .
O1 Tb1 O2 78.47(6) . .
O1 Tb1 O2 78.47(6) 4_656 .
O1 Tb1 B2 101.53(6) 4_656 .
O1 Tb1 B2 101.53(6) . .
O1 Tb1 B1 92.5(4) 4_656 4_656
O1 Tb1 B1 88.0(5) 4_656 .
O1 Tb1 B1 88.0(5) . 4_656
O1 Tb1 B1 92.5(4) . .
O1 Tb1 I2A 90.36(12) 4_656 .
O1 Tb1 I2A 90.36(12) . 4_656
O1 Tb1 I2A 87.31(12) 4_656 4_656
O1 Tb1 I2A 87.31(12) . .
O2 Tb1 B2 180.0 . .
O2 Tb1 B1 91.1(3) . .
O2 Tb1 B1 91.1(3) . 4_656
O2 Tb1 I2A 84.17(8) . 4_656
O2 Tb1 I2A 84.17(8) . .
B2 Tb1 I2A 95.83(8) . 4_656
B2 Tb1 I2A 95.83(8) . .
B1 Tb1 B2 88.9(3) 4_656 .
B1 Tb1 B2 88.9(3) . .
B1 Tb1 B1 177.7(6) . 4_656
B1 Tb1 I2A 8.0(3) 4_656 4_656
B1 Tb1 I2A 173.9(5) . 4_656
I2A Tb1 I2A 168.34(17) . 4_656
C1 O1 Tb1 127.0(2) . .
C4 O1 Tb1 124.5(2) . .
C4 O1 C1 108.3(3) . .
C5 O2 Tb1 126.1(2) . .
C5 O2 Tb1 126.1(2) 4_656 .
C5 O2 C5 107.8(4) . 4_656
O1 C1 C2 106.1(3) . .
C3 C2 C1 104.2(4) . .
C4 C3 C2 104.0(4) . .
O1 C4 C3 105.9(3) . .
O2 C5 C6 105.4(4) . .
C6 C6 C5 102.4(4) 4_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O1 2.358(3) 4_656
Tb1 O1 2.358(2) .
Tb1 O2 2.434(3) .
Tb1 B2 2.733(6) .
Tb1 B1 2.686(14) .
Tb1 B1 2.686(14) 4_656
Tb1 I2A 2.874(4) .
Tb1 I2A 2.874(4) 4_656
O1 C1 1.468(4) .
O1 C4 1.461(5) .
O2 C5 1.457(5) .
O2 C5 1.457(5) 4_656
C1 C2 1.502(6) .
C2 C3 1.498(7) .
C3 C4 1.477(6) .
C5 C6 1.494(7) .
C6 C6 1.485(12) 4_656
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
12.0000 -8.0000 -0.0000 -0.3487 -0.9371 -0.1287
-7.0000 -16.0000 1.0000 0.1045 0.2856 -0.9123
5.0000 -18.0000 1.0000 -0.2286 -0.5708 -0.7550
-2.0000 20.0000 -1.0000 0.1518 0.3903 0.9135
-13.0000 5.0000 0.0000 0.3682 0.9658 -0.0354
11.0000 2.0000 -10.0000 0.1550 -0.9041 0.3503
10.0000 -6.0000 -10.0000 0.1615 -0.9426 -0.0521
-11.0000 5.0000 11.0000 -0.1818 1.0153 -0.0190
-6.0000 -17.0000 4.0000 -0.0605 0.2542 -0.9459
4.0000 13.0000 15.0000 -0.7510 0.1545 0.6687
-1.0000 4.0000 -20.0000 0.9385 -0.2184 0.2164
3.0000 19.0000 -7.0000 0.2828 -0.0711 0.9851
4.0000 19.0000 1.0000 -0.1048 -0.0037 0.9875
-3.0000 -19.0000 4.0000 -0.1477 0.0199 -0.9781
-6.0000 -11.0000 -14.0000 0.7658 0.0278 -0.6178
-8.0000 10.0000 -13.0000 0.8301 0.4657 0.3386
-11.0000 10.0000 -2.0000 0.4167 0.8607 0.2497
-9.0000 10.0000 12.0000 -0.2685 0.9614 0.2591
-10.0000 2.0000 12.0000 -0.2620 0.9229 -0.1433
-3.0000 5.0000 20.0000 -0.8058 0.6160 0.1283
5.0000 -14.0000 13.0000 -0.7586 -0.3121 -0.5925
9.0000 10.0000 11.0000 -0.7153 -0.2998 0.6403
8.0000 -6.0000 15.0000 -0.9098 -0.3777 -0.1527
8.0000 14.0000 8.0000 -0.5424 -0.2280 0.8170
9.0000 3.0000 -15.0000 0.4375 -0.8377 0.3676
8.0000 -5.0000 -15.0000 0.4440 -0.8762 -0.0348
5.0000 -14.0000 -12.0000 0.3674 -0.7388 -0.5339
6.0000 6.0000 -18.0000 0.6624 -0.6412 0.4544
4.0000 -6.0000 -19.0000 0.7308 -0.6815 -0.1573
-5.0000 9.0000 17.0000 -0.6056 0.7568 0.2839
1.0000 -4.0000 20.0000 -0.9385 0.2184 -0.2164
3.0000 12.0000 16.0000 -0.7713 0.2272 0.5977
