#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:47:03 +0100 (jue 07 de nov de 2019) $
#$Revision: 224104 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/95/7049540.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_7049540
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 Yb'
_chemical_formula_weight         795.68
_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                   13.8721(8)
_cell_length_b                   13.8721(8)
_cell_length_c                   15.0022(18)
_cell_measurement_reflns_used    4387
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.79
_cell_measurement_theta_min      2.72
_cell_volume                     2500.2(4)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0617
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19615
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         2.172
_exptl_absorpt_coefficient_mu    1.972
_exptl_absorpt_correction_T_max  0.6282
_exptl_absorpt_correction_T_min  0.5711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.057
_exptl_crystal_description       block
_exptl_crystal_F_000             814
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.894
_refine_diff_density_min         -2.968
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         966
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0756
_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)+(0.1507P)²+4.7662P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2339
_refine_ls_wR_factor_ref         0.2410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                818
_reflns_number_total             966
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00663j2.cif
_cod_data_source_block           1-Yb
_cod_depositor_comments
'Adding full bibliography for 7049540--7049541.cif.'
_cod_database_code               7049540
_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   0.537
_shelx_estimated_absorpt_t_max   0.589
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -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
Yb1 Yb 0.666667 0.333333 0.250000 0.0710(6) Uani 1 12 d S TU P
P1 P 0.666667 0.333333 0.0063(6) 0.0831(14) Uani 1 6 d S TU P
O1 O 0.666667 0.333333 0.1121(12) 0.071(3) Uani 1 6 d S TU P
O2 O 0.5006(10) 0.3443(10) 0.250000 0.126(4) Uani 1 2 d S TU P
O3 O 0.4982(7) 0.5018(7) 0.250000 0.143(7) Uani 1 4 d S T P
N1 N 0.5485(6) 0.4515(6) 0.250000 0.110(4) Uani 1 4 d S TU P
C1 C 0.7403(6) 0.2597(6) -0.0406(13) 0.139(6) Uani 1 2 d DS TU P
C2 C 0.7495(10) 0.2505(10) -0.1419(13) 0.169(7) Uani 1 2 d DS TU P
H2A H 0.788342 0.211658 -0.155726 0.253 Uiso 1 2 d R U P
H2B H 0.676032 0.215040 -0.166446 0.253 Uiso 1 1 d R U .
C3 C 0.8505(11) 0.3065(15) 0.0089(14) 0.176(6) Uani 1 1 d D U .
H3A H 0.839700 0.317838 0.070421 0.264 Uiso 1 1 calc R U .
H3B H 0.903788 0.376209 -0.017288 0.264 Uiso 1 1 calc R U .
H3C H 0.877442 0.254983 0.004883 0.264 Uiso 1 1 calc 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'
O O 0.0106 0.0060 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 '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 Yb1 O1 180.0 16_556 .
O1 Yb1 O2 90.002(2) 16_556 20_655
O1 Yb1 O2 90.000(2) . 20_655
O1 Yb1 O2 90.002(1) 16_556 2_655
O1 Yb1 O2 90.000(1) . 2_655
O2 Yb1 O2 66.3(6) 20_655 2_655
O1 Yb1 O2 90.000(2) 16_556 3_665
O1 Yb1 O2 90.000(2) . 3_665
O2 Yb1 O2 53.7(6) 20_655 3_665
O2 Yb1 O2 120.002(1) 2_655 3_665
O1 Yb1 O2 90.000(2) 16_556 21
O1 Yb1 O2 90.000(2) . 21
O2 Yb1 O2 120.002(1) 20_655 21
O2 Yb1 O2 53.7(6) 2_655 21
O2 Yb1 O2 173.7(6) 3_665 21
O1 Yb1 O2 89.998(1) 16_556 .
O1 Yb1 O2 90.000(2) . .
O2 Yb1 O2 173.7(6) 20_655 .
O2 Yb1 O2 119.999(2) 2_655 .
O2 Yb1 O2 119.999(1) 3_665 .
O2 Yb1 O2 66.3(6) 21 .
O1 Yb1 O2 89.998(1) 16_556 19_665
O1 Yb1 O2 90.000(1) . 19_665
O2 Yb1 O2 120.000(3) 20_655 19_665
O2 Yb1 O2 173.7(6) 2_655 19_665
O2 Yb1 O2 66.3(6) 3_665 19_665
O2 Yb1 O2 119.998(2) 21 19_665
O2 Yb1 O2 53.7(6) . 19_665
O1 Yb1 N1 90.001(2) 16_556 3_665
O1 Yb1 N1 90.000(2) . 3_665
O2 Yb1 N1 26.8(3) 20_655 3_665
O2 Yb1 N1 93.2(3) 2_655 3_665
O2 Yb1 N1 26.8(3) 3_665 3_665
O2 Yb1 N1 146.8(3) 21 3_665
O2 Yb1 N1 146.8(3) . 3_665
O2 Yb1 N1 93.2(3) 19_665 3_665
O1 Yb1 N1 90.001(2) 16_556 2_655
O1 Yb1 N1 90.000(2) . 2_655
O2 Yb1 N1 93.2(3) 20_655 2_655
O2 Yb1 N1 26.8(3) 2_655 2_655
O2 Yb1 N1 146.8(3) 3_665 2_655
O2 Yb1 N1 26.8(3) 21 2_655
O2 Yb1 N1 93.2(3) . 2_655
O2 Yb1 N1 146.8(3) 19_665 2_655
N1 Yb1 N1 120.0 3_665 2_655
O1 P1 C1 111.7(6) . .
O1 P1 C1 111.7(6) . 3_665
C1 P1 C1 107.2(7) . 3_665
O1 P1 C1 111.7(6) . 2_655
C1 P1 C1 107.2(7) . 2_655
C1 P1 C1 107.2(7) 3_665 2_655
P1 O1 Yb1 180.0 . .
N1 O2 Yb1 96.6(9) . .
O3 N1 O2 123.5(8) . 19_665
O3 N1 O2 123.5(8) . .
O2 N1 O2 113.1(15) 19_665 .
C3 C1 C3 91.4(17) . 19_665
C3 C1 C2 114.3(10) . .
C3 C1 C2 114.3(10) 19_665 .
C3 C1 P1 106.5(10) . .
C3 C1 P1 106.5(10) 19_665 .
C2 C1 P1 119.9(13) . .
C1 C2 H2A 110.8 . .
C1 C2 H2B 108.3 . .
H2A C2 H2B 112.4 . .
C1 C2 H2B 108.3(6) . 19_665
H2A C2 H2B 112.4 . 19_665
H2B C2 H2B 104.4 . 19_665
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Yb1 O1 2.069(18) 16_556
Yb1 O1 2.069(18) .
Yb1 O2 2.384(12) 20_655
Yb1 O2 2.384(12) 2_655
Yb1 O2 2.384(12) 3_665
Yb1 O2 2.384(12) 21
Yb1 O2 2.384(12) .
Yb1 O2 2.384(12) 19_665
Yb1 N1 2.839(14) 3_665
Yb1 N1 2.839(14) 2_655
P1 O1 1.59(2) .
P1 C1 1.904(14) .
P1 C1 1.904(14) 3_665
P1 C1 1.904(14) 2_655
O2 N1 1.290(13) .
O3 N1 1.21(2) .
C1 C3 1.522(9) .
C1 C3 1.522(9) 19_665
C1 C2 1.536(9) .
C2 H2A 0.9573 .
C2 H2B 0.9562 .
C2 H2B 0.9561 19_665
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
