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_7040906
_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
'C16 H16 Cl Mo2 N4 O4 S4, C5 H6 N, 1.5(C5 H5 N)'
_chemical_formula_sum            'C28.5 H29.5 Cl Mo2 N6.5 O4 S4'
_chemical_formula_weight         882.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 92.425(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.762(3)
_cell_length_b                   14.296(5)
_cell_length_c                   26.630(8)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.33
_cell_volume                     3332.7(19)
_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  'XL (Sheldrick, 2008)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            64686
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.601
_diffrn_reflns_theta_min         1.531
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.129
_exptl_absorpt_correction_T_max  0.9820
_exptl_absorpt_correction_T_min  0.8621
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0940 before and 0.0489 after correction.
The Ratio of minimum to maximum transmission is 0.8779.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         7714
_refine_ls_number_restraints     429
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0284P)^2^+8.9555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6300
_reflns_number_total             7714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03659g2.cif
_cod_data_source_block           2-py
_cod_depositor_comments
'Adding full bibliography for 7040905--7040906.cif.'
_cod_original_cell_volume        3332.8(19)
_cod_original_formula_sum        'C28.50 H29.50 Cl Mo2 N6.50 O4 S4'
_cod_database_code               7040906
_shelxl_version_number           2014-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
N5 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim N5A \\sim C17A \\sim
C18A \\sim C19A \\sim C20A \\sim C21A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
N6 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim N6A \\sim C22A \\sim
C23A \\sim C24A \\sim C25A \\sim C26A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Same fragment restrains
{N5A, C17A, C18A, C19A, C20A, C21A} sigma for 1-2: 0.02, 1-3: 0.04
{N6, C22, C23, C24, C25, C26} sigma for 1-2: 0.02, 1-3: 0.04
{N6A, C22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
{N7, C27, C28, C29, C30, C31} sigma for 1-2: 0.02, 1-3: 0.04
as
{N5, C17, C18, C19, C20, C21}
4. Others
 Sof(N5A)=Sof(H5A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=
 Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=1-FVAR(1)
 Sof(N5)=Sof(H5)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=
 Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=FVAR(1)
 Sof(N6A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=1-FVAR(2)
 Sof(N6)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=FVAR(2)
 Fixed Sof: N7(0.5) C27(0.5) H27(0.5) C28(0.5) H28(0.5) C29(0.5) H29(0.5)
 C30(0.5) H30(0.5) C31(0.5) H31(0.5)
5.a Ternary CH refined with riding coordinates:
 C18A(H18A)
5.b 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)
5.c Aromatic/amide H refined with riding coordinates:
 N5(H5), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), N5A(H5A),
 C17A(H17A), C19A(H19A), C20A(H20A), C21A(H21A), C22(H22), C23(H23), C24(H24),
 C25(H25), C26(H26), C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31)
;
_shelx_res_checksum              49480
_olex2_submission_special_instructions 'No special instructions were received'