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_7704323
_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
'C36 H48 Co9 N12 Na14 O179 P12 Se4 W24, 23(O)'
_chemical_formula_sum            'C36 H48 Co9 N12 Na14 O202 P12 Se4 W24'
_chemical_formula_weight         9832.97
_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.cc23h17x
_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                85.5630(10)
_cell_angle_beta                 86.4740(10)
_cell_angle_gamma                62.9300(10)
_cell_formula_units_Z            1
_cell_length_a                   18.1321(14)
_cell_length_b                   18.8474(14)
_cell_length_c                   20.3150(15)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.32
_cell_volume                     6160.7(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0923
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31999
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.534
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.543
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1372 before and 0.0515 after correction. The Ratio of minimum to maximum transmission is 0.4444. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.650
_exptl_crystal_description       block
_exptl_crystal_F_000             4453
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.874
_refine_diff_density_min         -4.915
_refine_diff_density_rms         0.339
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1358
_refine_ls_number_reflns         21771
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0916P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15657
_reflns_number_total             21771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00444h2.cif
_cod_data_source_block           1950868
_cod_depositor_comments
'Adding full bibliography for 7704323--7704325.cif.'
_cod_database_code               7704323
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.211
_shelx_estimated_absorpt_t_min   0.079
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Shared sites
{Co5, Na1}
{Co6, Na2}
3. Uiso/Uaniso restraints and constraints
Uanis(O34) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(O12W)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(O2) \\sim Ueq,
Uanis(O11) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(O22W) \\sim Ueq, Uanis(O31W)
\\sim Ueq, Uanis(O21W) \\sim Ueq, Uanis(O30W) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uiso(Co5) = Uiso(Na1)
Uiso(Co6) = Uiso(Na2)
4. Others
 Fixed Sof: O26W(0.5) O29W(0.5) Co5(0.2) Na1(0.3) O22W(0.5) O27W(0.5)
 O28W(0.5) Co6(0.3) Na2(0.7) O32W(0.5)
5.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              22615
_shelx_fab_checksum              48455
_olex2_submission_special_instructions 'No special instructions were received'