Selenotungstates incorporating organophosphonate ligands and metal ions: synthesis, characterization, magnetism and catalytic efficiency in the Knoevenagel condensation reaction.
Kong, Hui; He, Peipei; Yang, Zongfei; Xu, Qiaofei; Wang, Jiawei; Ban, Ran; Ma, Pengtao; Wang, Jingping; Niu, Jingyang; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7420–7425; doi:10.1039/d0dt00444h

data_7704325
_publ_section_title
;
 Selenotungstates incorporating organophosphonate ligands and metal ions:
 synthesis, characterization, magnetism and catalytic efficiency in the
 Knoevenagel condensation reaction.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7420
_journal_page_last               7425
_journal_paper_doi               10.1039/d0dt00444h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C18 H24 Cs2 N6 Na2 Ni4 O79 P6 Se2 W12, 11(O)'
_chemical_formula_sum            'C18 H24 Cs2 N6 Na2 Ni4 O90 P6 Se2 W12'
_chemical_formula_weight         4861.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc23h1h5
_audit_creation_date             2020-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-10 deposited with the CCDC.	2020-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.418(2)
_cell_angle_beta                 104.442(2)
_cell_angle_gamma                111.826(2)
_cell_formula_units_Z            2
_cell_length_a                   16.9074(19)
_cell_length_b                   19.793(2)
_cell_length_c                   24.551(3)
_cell_measurement_reflns_used    7135
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.23
_cell_measurement_theta_min      2.39
_cell_volume                     7340.1(14)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0444
_diffrn_reflns_av_unetI/netI     0.1135
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38211
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.724
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.998
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0935 before and 0.0448 after correction. The Ratio of minimum to maximum transmission is 0.6686. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.199
_exptl_crystal_description       block
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.235
_refine_diff_density_min         -1.809
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1218
_refine_ls_number_reflns         25983
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0554
_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/[\s^2^(Fo^2^)+(0.0655P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13620
_reflns_number_total             25983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00444h2.cif
_cod_data_source_block           1950876
_cod_depositor_comments
'Adding full bibliography for 7704323--7704325.cif.'
_cod_original_cell_volume        7340.0(14)
_cod_database_code               7704325
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.206
_shelx_estimated_absorpt_t_min   0.110
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C11-C12 = C11-N4 = C2-C3
 1.47 with sigma of 0.01
 C2-N1
 1.47 with sigma of 0.02
 C17-N6
 1.47 with sigma of 0.02
 O3W-O14 = O2W-O51
 2.6 with sigma of 0.04
3. Rigid bond restraints
 O35, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O33, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O69, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 W11, O63
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O32, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O65, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(O32)
\\sim Ueq, Uanis(O37) \\sim Ueq, Uanis(O69) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Ni4(0.65) Ni5(0.35)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B),
 C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B),
  C17(H17A,H17B)
;
_shelx_res_checksum              34386
_shelx_fab_checksum              30826
_olex2_submission_special_instructions 'No special instructions were received'