A series of Keggin-based compounds constructed by conjugate ring-rich pyrazine and quinoxaline derivatives.
Tian, Aixiang; Tian, Yan; Ning, Yali; Hou, Xue; Ni, Huaiping; Ji, Xuebin; Liu, Guocheng; Ying, Jun; Dalton transactions (Cambridge, England : 2003) 45 (2016) 13925–13936; doi:10.1039/c6dt02233b

data_7040070
_publ_section_title
;
 A series of Keggin-based compounds constructed by conjugate ring-rich
 pyrazine and quinoxaline derivatives.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13925
_journal_page_last               13936
_journal_paper_doi               10.1039/c6dt02233b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'0.5(C80 H56 Ag4 Mo24 N8 O80 Si2), 2(C16 H36 N)'
_chemical_formula_sum            'C72 H100 Ag2 Mo12 N6 O40 Si'
_chemical_formula_weight         3084.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-12 deposited with the CCDC.
2016-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.1530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.9259(6)
_cell_length_b                   13.7086(5)
_cell_length_c                   21.2814(8)
_cell_measurement_reflns_used    7629
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      1.71
_cell_volume                     4844.7(3)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35534
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.346
_diffrn_reflns_theta_min         1.708
_exptl_absorpt_coefficient_mu    1.987
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.115
_exptl_crystal_description       block
_exptl_crystal_F_000             3012
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.862
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         12094
_refine_ls_number_restraints     714
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0265P)^2^+23.2943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8501
_reflns_number_total             12094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02233b2.cif
_cod_data_source_block           compound-4
_cod_depositor_comments
'Adding full bibliography for 7040067--7040071.cif.'
_cod_database_code               7040070
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C34A-C35A = C34-C35
 1.57 with sigma of 0.01
 C25-C26
 1.57 with sigma of 0.01
 C34-C33 \\sim C33-C34A
 with sigma of 0.02
 C34A-C35A \\sim C34-C35
 with sigma of 0.02
 C35A-C36 \\sim C36-C35
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H30C)=Sof(H30D)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C31A)=
 Sof(H31C)=Sof(H31D)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C31)=Sof(H31A)=
 Sof(H31B)=FVAR(1)
 Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(2)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(H27A)=Sof(H27B)=FVAR(2)
 Sof(H33C)=Sof(H33D)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C35A)=Sof(H35C)=
 Sof(H35D)=Sof(C34A)=Sof(H34C)=Sof(H34D)=1-FVAR(3)
 Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=
 Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(3)
 Fixed Sof: O1(0.5) O1'(0.5) O2(0.5) O2'(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27C,H27D), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B),
 C30(H30C,H30D), C33(H33A,H33B), C33(H33C,H33D), C34(H34A,H34B), C35(H35A,H35B),
  C31(H31A,H31B), C31A(H31C,H31D), C35A(H35C,H35D), C34A(H34C,H34D)
6.b Me refined with riding coordinates:
 C36(H36A,H36B,H36C), C36(H36D,H36E,H36F)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
6.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C32A(H32D,H32E,
 H32F), C28A(H28D,H28E,H28F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'