K3[Mo2(SNO5)4Cl]3[Mo2(SNO5)4]: the first example of a heterometallic extended metal atom node (HEMAN).
Dolinar, Brian S.; Kozimor, Stosh A.; Berry, John F.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17602–17605; doi:10.1039/c6dt03659g

data_7040905
_publ_section_title
;
 K3[Mo2(SNO5)4Cl]3[Mo2(SNO5)4]: the first example of a heterometallic
 extended metal atom node (HEMAN).
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17602
_journal_page_last               17605
_journal_paper_doi               10.1039/c6dt03659g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '2(C32 H32 Cl1.5 K1.5 Mo4 N8 O8 S8), 0.5(O)'
_chemical_formula_sum            'C64 H64 Cl3 K3 Mo8 N16 O16.5 S16'
_chemical_formula_weight         2825.44
_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             2015-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-08-03 deposited with the CCDC.
2016-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                88.31(3)
_cell_angle_beta                 79.279(18)
_cell_angle_gamma                63.20(2)
_cell_formula_units_Z            2
_cell_length_a                   16.397(7)
_cell_length_b                   17.295(6)
_cell_length_c                   24.416(13)
_cell_measurement_reflns_used    6871
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      23.619
_cell_measurement_theta_min      2.218
_cell_volume                     6061(5)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX2 Ver. 2014.1-1 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_av_unetI/netI     0.1344
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            57281
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.450
_diffrn_reflns_theta_min         1.322
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  0.4288
_exptl_absorpt_correction_T_min  0.3516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0922 before and 0.0466 after correction.
The Ratio of minimum to maximum transmission is 0.8200.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.519
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1151
_refine_ls_number_reflns         22344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0675
_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^)+(0.0876P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11517
_reflns_number_total             22344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03659g2.cif
_cod_data_source_block           1-10MeCN
_cod_depositor_comments
'Adding full bibliography for 7040905--7040906.cif.'
_cod_original_formula_sum        'C64 H64 Cl3 K3 Mo8 N16 O16.50 S16'
_cod_database_code               7040905
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Fixed Sof: Cl1(0.5) Cl1A(0.5) O1S(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B), C11(H11A,
 H11B), C14(H14A,H14B), C15(H15A,H15B), C18(H18A,H18B), C19(H19A,H19B),
 C22(H22A,H22B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B), C30(H30A,H30B),
  C31(H31A,H31B), C2A(H2AA,H2AB), C3A(H3AA,H3AB), C6A(H6AA,H6AB), C7A(H7AA,
 H7AB), C10A(H10C,H10D), C11A(H11C,H11D), C14A(H14C,H14D), C15A(H15C,H15D),
 C18A(H18C,H18D), C19A(H19C,H19D), C22A(H22C,H22D), C23A(H23C,H23D), C26A(H26C,
 H26D), C27A(H27C,H27D), C30A(H30C,H30D), C31A(H31C,H31D)
;
_shelx_res_checksum              62660
_olex2_submission_special_instructions 'No special instructions were received'