#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:03:03 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223689 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/26/7232603.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_7232603
loop_
_publ_author_name
'Zhao, Yanxin'
'Chen, Shumin'
'Ji, Yanfang'
'Singh, Vikram'
'Ma, Pengtao'
'Lu, Jingkun'
'Niu, Jingyang'
'Wang, Jingping'
_publ_section_title
;
 Ln(iii)-Containing polyoxomolybdates based on β-{Mo8O28}: microwave
 synthesis and optical and magnetic properties
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              3627
_journal_paper_doi               10.1039/C9CE00229D
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'Mo8 O37 Tm2, 8(O)'
_chemical_formula_sum            'Mo8 O45 Tm2'
_chemical_formula_weight         1825.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-04 deposited with the CCDC.    2019-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.6230(10)
_cell_angle_beta                 99.0190(10)
_cell_angle_gamma                102.6890(10)
_cell_formula_units_Z            1
_cell_length_a                   9.2867(7)
_cell_length_b                   10.2931(8)
_cell_length_c                   10.7281(8)
_cell_measurement_reflns_used    4304
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.69
_cell_volume                     986.98(13)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5070
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.096
_diffrn_reflns_theta_max         25.096
_diffrn_reflns_theta_min         2.030
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.018
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0916 before and 0.0269 after correction. The Ratio of minimum to maximum transmission is 0.6295. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.071
_exptl_crystal_description       block
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.036
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0285P)²+6.8691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3303
_reflns_number_total             3463
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce00229d2.cif
_cod_data_source_block           njy1_a
_cod_depositor_comments
'Adding full bibliography for 7232603--7232604.cif.'
_cod_database_code               7232603
_shelx_shelxl_version_number     2018/1
_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_max   0.419
_shelx_estimated_absorpt_t_min   0.295
_olex2_refinement_description
;
1. Others
 Fixed Sof: O9W(0.5) O10W(0.5)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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
Tm1 Tm 0.39055(3) 0.60909(2) 0.28734(2) 0.01504(9) Uani 1 1 d . . .
Mo1 Mo -0.13773(5) 0.95060(5) 0.59384(5) 0.01107(12) Uani 1 1 d . . .
Mo2 Mo 0.36284(5) 0.85821(5) 0.55526(5) 0.01223(12) Uani 1 1 d . . .
Mo3 Mo -0.22002(5) 0.86218(5) 0.29270(5) 0.01248(12) Uani 1 1 d . . .
Mo4 Mo 0.03823(5) 0.70308(5) 0.40069(5) 0.01262(12) Uani 1 1 d . . .
O1 O 0.0128(5) 0.9651(4) 0.7168(4) 0.0175(9) Uani 1 1 d . . .
O2 O -0.2701(5) 0.8221(4) 0.6335(4) 0.0210(9) Uani 1 1 d . . .
O3 O -0.2058(4) 1.1045(4) 0.6251(4) 0.0134(8) Uani 1 1 d . . .
O4 O -0.2520(4) 0.9886(4) 0.4110(4) 0.0142(8) Uani 1 1 d . . .
O5 O -0.0556(4) 0.8656(4) 0.4657(4) 0.0136(8) Uani 1 1 d . . .
O6 O -0.3623(5) 0.7283(4) 0.3181(4) 0.0214(10) Uani 1 1 d . . .
O7 O -0.2849(5) 0.9153(5) 0.1502(4) 0.0282(11) Uani 1 1 d . . .
O8 O -0.0815(4) 0.7611(4) 0.2509(4) 0.0149(8) Uani 1 1 d . . .
O9 O -0.1013(5) 0.5802(4) 0.4386(4) 0.0207(9) Uani 1 1 d . . .
O10 O 0.1637(4) 0.7406(4) 0.5588(4) 0.0154(9) Uani 1 1 d . . .
O11 O 0.1459(4) 0.6221(4) 0.3217(4) 0.0181(9) Uani 1 1 d . . .
O12 O 0.4342(5) 0.8496(5) 0.7097(4) 0.0235(10) Uani 1 1 d . . .
O13 O 0.500000 1.000000 0.500000 0.0198(13) Uani 1 2 d S T P
O14 O 0.4170(4) 0.7309(4) 0.4749(4) 0.0180(9) Uani 1 1 d . . .
O1W O 0.3332(5) 0.4491(4) 0.4353(4) 0.0246(10) Uani 1 1 d . . .
O2W O 0.5364(5) 0.4482(4) 0.2848(5) 0.0254(10) Uani 1 1 d . . .
O3W O 0.3554(6) 0.8084(5) 0.2080(5) 0.0306(11) Uani 1 1 d . . .
O4W O 0.2177(6) 0.4423(5) 0.1614(5) 0.0353(12) Uani 1 1 d . . .
O5W O 0.4492(6) 0.6114(5) 0.0797(4) 0.0286(11) Uani 1 1 d . . .
O6W O 0.7564(6) 0.4979(6) 0.1357(5) 0.0434(14) Uani 1 1 d . . .
O7W O 0.9388(7) 0.3240(7) 0.2130(6) 0.0550(17) Uani 1 1 d . . .
O8W O 0.3503(9) 0.2409(7) 0.0841(6) 0.0624(19) Uani 1 1 d . . .
O9W O 0.0073(19) 0.8604(16) 0.0123(16) 0.076(4) Uiso 0.5 1 d . . .
O10W O 0.3484(19) 0.8661(16) -0.0307(16) 0.077(4) Uiso 0.5 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo Mo -1.6832 0.6857 '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'
Tm Tm -0.3139 5.2483 '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
O6 Tm1 O11 142.48(14) 1_655 .
O6 Tm1 O1W 115.14(16) 1_655 .
O6 Tm1 O2W 74.32(16) 1_655 .
O6 Tm1 O4W 143.53(16) 1_655 .
O6 Tm1 O5W 77.55(17) 1_655 .
O14 Tm1 O6 75.99(15) . 1_655
O14 Tm1 O11 72.44(14) . .
O14 Tm1 O1W 75.43(16) . .
O14 Tm1 O2W 116.95(16) . .
O14 Tm1 O4W 140.01(16) . .
O14 Tm1 O5W 145.63(16) . .
O1W Tm1 O11 75.80(15) . .
O1W Tm1 O2W 69.31(16) . .
O1W Tm1 O5W 136.62(16) . .
O2W Tm1 O11 138.98(15) . .
O2W Tm1 O5W 75.70(16) . .
O3W Tm1 O6 80.64(17) . 1_655
O3W Tm1 O11 74.75(16) . .
O3W Tm1 O14 80.66(16) . .
O3W Tm1 O1W 146.45(16) . .
O3W Tm1 O2W 143.83(17) . .
O3W Tm1 O4W 106.5(2) . .
O3W Tm1 O5W 73.70(17) . .
O4W Tm1 O11 71.87(16) . .
O4W Tm1 O1W 78.87(18) . .
O4W Tm1 O2W 80.69(18) . .
O4W Tm1 O5W 70.75(18) . .
O5W Tm1 O11 120.52(16) . .
O1 Mo1 O3 101.24(18) . .
O1 Mo1 O4 156.23(18) . .
O1 Mo1 O5 97.99(18) . .
O1 Mo1 O5 75.87(17) . 2_576
O2 Mo1 O1 104.2(2) . .
O2 Mo1 O3 104.99(19) . .
O2 Mo1 O4 99.18(19) . .
O2 Mo1 O5 102.33(19) . .
O2 Mo1 O5 179.10(18) . 2_576
O3 Mo1 O4 76.44(16) . .
O3 Mo1 O5 141.30(17) . .
O3 Mo1 O5 75.85(15) . 2_576
O4 Mo1 O5 80.69(14) . 2_576
O5 Mo1 O4 72.56(15) . .
O5 Mo1 O5 76.78(16) . 2_576
O4 Mo2 O3 68.56(14) 2_576 2_576
O10 Mo2 O3 72.93(15) . 2_576
O10 Mo2 O4 83.29(16) . 2_576
O12 Mo2 O3 160.77(18) . 2_576
O12 Mo2 O4 94.32(19) . 2_576
O12 Mo2 O10 97.1(2) . .
O12 Mo2 O13 103.61(16) . .
O12 Mo2 O14 105.4(2) . .
O13 Mo2 O3 83.52(10) . 2_576
O13 Mo2 O4 82.80(11) . 2_576
O13 Mo2 O10 155.76(12) . .
O14 Mo2 O3 91.38(17) . 2_576
O14 Mo2 O4 159.94(18) . 2_576
O14 Mo2 O10 90.62(18) . .
O14 Mo2 O13 95.73(14) . .
O4 Mo3 O1 80.05(16) . 2_576
O4 Mo3 O5 72.44(15) . .
O4 Mo3 O8 144.73(17) . .
O5 Mo3 O1 71.52(14) . 2_576
O6 Mo3 O1 172.64(18) . 2_576
O6 Mo3 O4 98.24(19) . .
O6 Mo3 O5 101.13(18) . .
O6 Mo3 O8 97.75(19) . .
O7 Mo3 O1 83.4(2) . 2_576
O7 Mo3 O4 104.0(2) . .
O7 Mo3 O5 154.9(2) . .
O7 Mo3 O6 103.9(2) . .
O7 Mo3 O8 102.4(2) . .
O8 Mo3 O1 80.09(16) . 2_576
O8 Mo3 O5 73.74(15) . .
O5 Mo4 O3 74.39(14) . 2_576
O8 Mo4 O3 82.96(16) . 2_576
O8 Mo4 O5 72.72(15) . .
O9 Mo4 O3 168.14(18) . 2_576
O9 Mo4 O5 94.11(18) . .
O9 Mo4 O8 96.57(19) . .
O9 Mo4 O10 100.48(19) . .
O9 Mo4 O11 105.5(2) . .
O10 Mo4 O3 75.57(16) . 2_576
O10 Mo4 O5 82.65(16) . .
O10 Mo4 O8 150.92(17) . .
O11 Mo4 O3 86.30(17) . 2_576
O11 Mo4 O5 159.36(18) . .
O11 Mo4 O8 98.13(18) . .
O11 Mo4 O10 99.79(19) . .
Mo1 O1 Mo3 116.4(2) . 2_576
Mo1 O3 Mo2 108.18(18) . 2_576
Mo1 O3 Mo4 113.14(18) . 2_576
Mo4 O3 Mo2 90.23(14) 2_576 2_576
Mo2 O4 Mo1 105.57(17) 2_576 .
Mo3 O4 Mo1 106.83(17) . .
Mo3 O4 Mo2 147.4(2) . 2_576
Mo1 O5 Mo1 103.22(16) . 2_576
Mo1 O5 Mo3 103.45(16) . .
Mo1 O5 Mo4 151.1(2) . .
Mo3 O5 Mo1 95.97(15) . 2_576
Mo4 O5 Mo1 96.02(14) . 2_576
Mo4 O5 Mo3 95.65(15) . .
Mo3 O6 Tm1 153.1(3) . 1_455
Mo3 O8 Mo4 113.6(2) . .
Mo4 O10 Mo2 115.1(2) . .
Mo4 O11 Tm1 147.2(2) . .
Mo2 O13 Mo2 180.00(2) . 2_676
Mo2 O14 Tm1 146.7(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tm1 O6 2.323(4) 1_655
Tm1 O11 2.389(4) .
Tm1 O14 2.310(4) .
Tm1 O1W 2.335(4) .
Tm1 O2W 2.361(4) .
Tm1 O3W 2.299(5) .
Tm1 O4W 2.326(5) .
Tm1 O5W 2.374(5) .
Mo1 O1 1.744(4) .
Mo1 O2 1.704(4) .
Mo1 O3 1.876(4) .
Mo1 O4 2.162(4) .
Mo1 O5 1.958(4) .
Mo1 O5 2.471(4) 2_576
Mo2 O3 2.322(4) 2_576
Mo2 O4 2.120(4) 2_576
Mo2 O10 1.982(4) .
Mo2 O12 1.696(4) .
Mo2 O13 1.8822(5) .
Mo2 O14 1.765(4) .
Mo3 O1 2.332(4) 2_576
Mo3 O4 1.909(4) .
Mo3 O5 2.206(4) .
Mo3 O6 1.744(4) .
Mo3 O7 1.695(4) .
Mo3 O8 1.923(4) .
Mo4 O3 2.283(4) 2_576
Mo4 O5 2.202(4) .
Mo4 O8 1.982(4) .
Mo4 O9 1.703(4) .
Mo4 O10 1.884(4) .
Mo4 O11 1.741(4) .
