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_7040068
_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         'C80 H60 Mo16 N10 O40 Si'
_chemical_formula_sum            'C80 H60 Mo16 N10 O40 Si'
_chemical_formula_weight         3364.51
_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_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                111.8830(10)
_cell_angle_beta                 94.9400(10)
_cell_angle_gamma                107.6620(10)
_cell_formula_units_Z            2
_cell_length_a                   17.9317(8)
_cell_length_b                   18.5613(9)
_cell_length_c                   20.1606(10)
_cell_measurement_reflns_used    4886
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.27
_cell_volume                     5780.7(5)
_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)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.999
_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  0.0409
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33695
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.407
_exptl_absorpt_coefficient_mu    1.756
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_description       block
_exptl_crystal_F_000             3231
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.008
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1324
_refine_ls_number_reflns         20402
_refine_ls_number_restraints     1899
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0897P)^2^+1.8562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12696
_reflns_number_total             20402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02233b2.cif
_cod_data_source_block           compound-2
_cod_depositor_comments
'Adding full bibliography for 7040067--7040071.cif.'
_cod_original_cell_volume        5780.6(5)
_cod_database_code               7040068
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.743
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. 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
3.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C51(H51), C50(H50), C67(H67), C1AA(H1AA), C22(H22), C75(H75),
 C69(H69), C79(H79), C70(H70), C37(H37), C66(H66), C5AA(H5AA), C73(H73),
 C45(H45), C76(H76), C71(H71), C49(H49), C78(H78), C29(H29), C6AA(H6AA),
 C46(H46), C59(H59), C36(H36), C16(H16), C10(H10), C48(H48), C63(H63), C72(H72),
  C77(H77), C4AA(H4AA), C39(H39), C24(H24), C11(H11), C43(H43), C53(H53),
 C42(H42), C2AA(H2AA), C41(H41), C30(H30), C57(H57), C14(H14), C47(H47),
 C40(H40), C61(H61), C27(H27), C19(H19), C60(H60), C32(H32), C25(H25), C31(H31),
  C62(H62), C3AA(H3AA), C54(H54), C13(H13), C17(H17), C55(H55), C56(H56),
 C2(H2), C7(H7)
;
_shelx_fab_checksum              62182
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'