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_7040071
_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         '2(Mo6 O20 P0.5), C60 H42 Cu3 N6'
_chemical_formula_sum            'C60 H42 Cu3 Mo12 N6 O40 P'
_chemical_formula_weight         2859.86
_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                79.5090(10)
_cell_angle_beta                 84.7310(10)
_cell_angle_gamma                88.4640(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2679(6)
_cell_length_b                   13.7650(6)
_cell_length_c                   23.3329(11)
_cell_measurement_reflns_used    5722
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      2.25
_cell_volume                     4172.2(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)'
_diffrn_ambient_temperature      293.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30427
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.957
_diffrn_reflns_theta_min         0.891
_exptl_absorpt_coefficient_mu    2.593
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.276
_exptl_crystal_description       block
_exptl_crystal_F_000             2740
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.164
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1138
_refine_ls_number_reflns         19921
_refine_ls_number_restraints     1272
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0461P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12992
_reflns_number_total             19921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02233b2.cif
_cod_data_source_block           compound-5
_cod_depositor_comments
'Adding full bibliography for 7040067--7040071.cif.'
_cod_database_code               7040071
_shelx_estimated_absorpt_t_max   0.697
_shelx_estimated_absorpt_t_min   0.639
_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. Others
 Fixed Sof: O1(0.5) O1'(0.5) O2(0.5) O2'(0.5) O21(0.5) O21'(0.5) O22(0.5)
 O22'(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C25(H25), C26(H26),
  C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C45(H45), C46(H46), C47(H47),
  C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56),
 C57(H57), C58(H58), C59(H59), C60(H60)
;
_shelx_fab_checksum              51305
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'