#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:47:03 +0200 (Thu, 07 Nov 2019) $
#$Revision: 224104 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/95/7049541.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_7049541
loop_
_publ_author_name
'Zhao, Wen'
'Cui, Huihui'
'Chen, Xiao-Yun'
'Yi, Gangji'
'Chen, Lei'
'Yuan, Aihua'
'Luo, Cheng-Lin'
_publ_section_title
;
 An eight-coordinate ytterbium complex with a hexagonal bipyramid geometry
 exhibiting field-induced single-ion magnet behaviour.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5621
_journal_page_last               5626
_journal_paper_doi               10.1039/c9dt00663j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C24 H54 N3 O11 P2 Tb'
_chemical_formula_weight         781.56
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-03-10 deposited with the CCDC.    2019-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.9163(14)
_cell_length_b                   13.9163(14)
_cell_length_c                   15.107(4)
_cell_measurement_reflns_used    9694
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.70
_cell_volume                     2533.7(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19257
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.162
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_T_max  0.6625
_exptl_absorpt_correction_T_min  0.5861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.024
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.300
_refine_diff_density_max         4.006
_refine_diff_density_min         -2.610
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         960
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0763
_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)+(0.1500P)²+3.3072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2075
_refine_ls_wR_factor_ref         0.2111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                857
_reflns_number_total             960
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00663j2.cif
_cod_data_source_block           2-Tb
_cod_depositor_comments
'Adding full bibliography for 7049540--7049541.cif.'
_cod_database_code               7049541
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.586
_shelx_estimated_absorpt_t_max   0.663
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-y, -x, -z+1/2'
'x-y, -y, -z'
'x, x-y, -z+1/2'
'y, x, -z'
'-x+y, y, -z+1/2'
'-x, -x+y, -z'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'y, x, z-1/2'
'-x+y, y, z'
'-x, -x+y, z-1/2'
'-y, -x, z'
'x-y, -y, z-1/2'
'x, x-y, z'
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
Tb1 Tb 0.333333 0.666667 0.250000 0.0513(5) Uani 1 12 d S T P
P1 P 0.333333 0.666667 0.0021(3) 0.0470(8) Uani 1 6 d S T P
O1 O 0.333333 0.666667 0.1077(8) 0.056(3) Uani 1 6 d S T P
O2 O 0.4994(9) 0.8471(8) 0.250000 0.116(4) Uani 1 2 d S TU P
O3 O 0.5030(5) 1.0060(10) 0.250000 0.136(5) Uani 1 4 d S T P
N1 N 0.4520(5) 0.9040(10) 0.250000 0.092(4) Uani 1 4 d S TU P
C1 C 0.2584(4) 0.5168(9) -0.0346(8) 0.074(3) Uani 1 2 d S T P
C2 C 0.3168(10) 0.4612(10) 0.0058(13) 0.139(5) Uani 1 1 d . U .
H2A H 0.347617 0.494693 0.061977 0.208 Uiso 1 1 calc R U .
H2B H 0.375329 0.469635 -0.032864 0.208 Uiso 1 1 calc DR U .
H2C H 0.264880 0.383672 0.014070 0.208 Uiso 1 1 calc R U .
C3 C 0.2517(8) 0.5033(16) -0.1442(13) 0.137(6) Uani 1 2 d S T P
H3A H 0.213034 0.425284 -0.159687 0.205 Uiso 1 2 d R U P
H3B H 0.212784 0.538390 -0.168087 0.205 Uiso 1 1 d R U .
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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 '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_
_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 180.0 . 14_566
O1 Tb1 O2 90.000(1) . 20
O1 Tb1 O2 90.001(1) 14_566 20
O1 Tb1 O2 90.000(2) . 3_665
O1 Tb1 O2 90.001(2) 14_566 3_665
O2 Tb1 O2 68.2(5) 20 3_665
O1 Tb1 O2 90.000(2) . 7_665
O1 Tb1 O2 90.000(2) 14_566 7_665
O2 Tb1 O2 120.000(2) 20 7_665
O2 Tb1 O2 51.8(5) 3_665 7_665
O1 Tb1 O2 90.0 . 14_566
O1 Tb1 O2 90.0 14_566 14_566
O2 Tb1 O2 171.8(5) 20 14_566
O2 Tb1 O2 120.000(3) 3_665 14_566
O2 Tb1 O2 68.2(5) 7_665 14_566
O1 Tb1 O2 90.000(2) . 9_565
O1 Tb1 O2 89.999(2) 14_566 9_565
O2 Tb1 O2 120.000(3) 20 9_565
O2 Tb1 O2 171.8(5) 3_665 9_565
O2 Tb1 O2 120.000(1) 7_665 9_565
O2 Tb1 O2 51.8(5) 14_566 9_565
O1 Tb1 O2 90.000(2) . .
O1 Tb1 O2 90.000(2) 14_566 .
O2 Tb1 O2 51.8(5) 20 .
O2 Tb1 O2 120.0 3_665 .
O2 Tb1 O2 171.8(5) 7_665 .
O2 Tb1 O2 120.000(1) 14_566 .
O2 Tb1 O2 68.2(5) 9_565 .
O1 Tb1 N1 90.000(3) . 3_665
O1 Tb1 N1 90.001(2) 14_566 3_665
O2 Tb1 N1 94.1(3) 20 3_665
O2 Tb1 N1 25.9(3) 3_665 3_665
O2 Tb1 N1 25.9(3) 7_665 3_665
O2 Tb1 N1 94.1(3) 14_566 3_665
O2 Tb1 N1 145.9(3) 9_565 3_665
O2 Tb1 N1 145.9(3) . 3_665
O1 Tb1 N1 90.0 . 14_566
O1 Tb1 N1 89.998(1) 14_566 14_566
O2 Tb1 N1 145.9(3) 20 14_566
O2 Tb1 N1 145.9(3) 3_665 14_566
O2 Tb1 N1 94.1(3) 7_665 14_566
O2 Tb1 N1 25.9(3) 14_566 14_566
O2 Tb1 N1 25.9(3) 9_565 14_566
O2 Tb1 N1 94.1(3) . 14_566
N1 Tb1 N1 120.0 3_665 14_566
O1 P1 C1 107.0(4) . 5_565
O1 P1 C1 107.0(4) . .
C1 P1 C1 111.8(4) 5_565 .
O1 P1 C1 107.0(4) . 3_665
C1 P1 C1 111.8(4) 5_565 3_665
C1 P1 C1 111.8(4) . 3_665
P1 O1 Tb1 180.0 . .
N1 O2 Tb1 97.1(8) . .
O3 N1 O2 123.0(6) . .
O3 N1 O2 123.0(6) . 20
O2 N1 O2 114.0(13) . 20
C2 C1 C2 105.9(14) . 20
C2 C1 C3 111.1(10) . .
C2 C1 C3 111.1(10) 20 .
C2 C1 P1 107.9(7) . .
C2 C1 P1 107.9(7) 20 .
C3 C1 P1 112.6(10) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C3 H3A 109.6 . .
C1 C3 H3B 109.3 . .
H3A C3 H3B 109.9 . .
C1 C3 H3B 109.3(4) . 20
H3A C3 H3B 109.4 . 20
H3B C3 H3B 109.4 . 20
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O1 2.149(12) .
Tb1 O1 2.149(12) 14_566
Tb1 O2 2.417(10) 20
Tb1 O2 2.417(10) 3_665
Tb1 O2 2.417(10) 7_665
Tb1 O2 2.417(10) 14_566
Tb1 O2 2.417(10) 9_565
Tb1 O2 2.417(10) .
Tb1 N1 2.860(12) 3_665
Tb1 N1 2.860(12) 14_566
P1 O1 1.597(13) .
P1 C1 1.890(11) 5_565
P1 C1 1.890(11) .
P1 C1 1.890(11) 3_665
O2 N1 1.260(11) .
O3 N1 1.230(16) .
C1 C2 1.504(12) .
C1 C2 1.504(12) 20
C1 C3 1.66(2) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 H3A 0.9690 .
C3 H3B 0.9619 .
C3 H3B 0.9619 20
