Discovery and isolation of the trans-isomers of two 1 : 2-type lanthanide-containing monolacunary Dawson-type tungstophosphates: [Ln(III)(α2-P2W17O61)2](17-) (Ln = La, Ce).
Wan, Rong; Ma, Pengtao; Han, Mengdan; Zhang, Dongdi; Zhang, Chao; Niu, Jingyang; Wang, Jingping; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5398–5405; doi:10.1039/c7dt00250e

data_7042583
_publ_section_title
;
 Discovery and isolation of the trans-isomers of two
 1&#x2009;:&#x2009;2-type lanthanide-containing monolacunary Dawson-type
 tungstophosphates: [Ln(III)(\a2-P2W17O61)2](17-) (Ln = La, Ce).
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5398
_journal_page_last               5405
_journal_paper_doi               10.1039/c7dt00250e
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'Ce O122 P4 W34, 9(C4 H12 N), 4(O)'
_chemical_formula_sum            'C36 H116 Ce N9 O126 P4 W34'
_chemical_formula_weight         9206.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-01-17 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.0880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.1944(13)
_cell_length_b                   32.1245(15)
_cell_length_c                   27.6417(13)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.83
_cell_measurement_theta_min      2.38
_cell_volume                     23200.8(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            59865
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.477
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.067
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1336 before and 0.0533 after correction.
The Ratio of minimum to maximum transmission is 0.4892.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.636
_exptl_crystal_description       block
_exptl_crystal_F_000             16148
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.352
_refine_diff_density_min         -1.632
_refine_diff_density_rms         0.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         20598
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+578.6161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1300
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13885
_reflns_number_total             20598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00250e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7042582--7042583.cif.'
_cod_database_code               7042583
_shelx_estimated_absorpt_t_max   0.124
_shelx_estimated_absorpt_t_min   0.054
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C1 = N1-C2 = N1-C3 = N1-C4
 1.5 with sigma of 0.02
 N2-C5 = N2-C6 = N2-C7 = N2-C8
 1.5 with sigma of 0.02
 N3-C9 = N3-C10
 1.5 with sigma of 0.02
 N4-C11 = N4-C12 = N4-C13 = N4-C14
 1.5 with sigma of 0.02
 N5-C15 = N5-C16 = N5-C17 = N5-C18
 1.5 with sigma of 0.02
 C1-C2 \\sim C1-C3 \\sim C1-C4 \\sim C2-C3 \\sim C2-C4 \\sim C3-C4
 with sigma of 0.02
 C5-C6 \\sim C5-C7 \\sim C5-C8 \\sim C6-C7 \\sim C6-C8 \\sim C7-C8
 with sigma of 0.02
 C11-C12 \\sim C11-C13 \\sim C11-C14 \\sim C12-C13 \\sim C12-C14 \\sim C13-C14
 with sigma of 0.02
 C15-C16 \\sim C15-C17 \\sim C15-C18 \\sim C16-C17 \\sim C16-C18 \\sim C17-C18
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(P2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Others
 Fixed Sof: O1W(0.5) O2W(0.5) O3W(0.7) O4W(0.3)
 Fixed Uiso: N4(0.12188) N5(0.12454) C4(0.10708) C7(0.13014) C8(0.12939)
 C10(0.1258) C11(0.12741) C12(0.15116) C13(0.1503) C14(0.14214) C15(0.12709)
 C16(0.13331) C17(0.15244) C18(0.13672)
5.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'