A dimolybdenum paddlewheel as a building block for heteromultimetallic structures.
Knöfel, Nicolai D; Schoo, Christoph; Seifert, Tim P.; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 1513–1521; doi:10.1039/c9dt04167b

data_7703258
_publ_section_title
;
 A dimolybdenum paddlewheel as a building block for heteromultimetallic
 structures.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1513
_journal_page_last               1521
_journal_paper_doi               10.1039/c9dt04167b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'0.5(C120 H112 Au8 Cl8 Mo4 O16 P8), 2(C4 H8 O), 4[C4H8O]'
_chemical_formula_sum            'C84 H104 Au4 Cl4 Mo2 O14 P4'
_chemical_formula_weight         2583.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-23
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5530)
;
_audit_update_record
;
2019-10-24 deposited with the CCDC.	2020-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6562(7)
_cell_length_b                   18.6547(7)
_cell_length_c                   24.8118(7)
_cell_measurement_reflns_used    16917
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      1.66
_cell_volume                     10023.7(6)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
 105 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1089
_diffrn_reflns_av_unetI/netI     0.1017
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31447
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.132
_diffrn_reflns_theta_min         1.658
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.299
_exptl_absorpt_correction_T_max  0.6459
_exptl_absorpt_correction_T_min  0.2172
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRED & LANA'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       plate
_exptl_crystal_F_000             4992
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.058
_refine_diff_density_max         2.786
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         9867
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.0737
_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^)+(0.1178P)^2^+48.7944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.2283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5107
_reflns_number_total             9867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04167b2.cif
_cod_data_source_block           nk122
_cod_depositor_comments
'Adding full bibliography for 7703254--7703259.cif.'
_cod_database_code               7703258
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C34-C33 \\sim C33-C32 \\sim C32-C31
 with sigma of 0.02
 O5-C34 \\sim O5-C31
 with sigma of 0.02
 O5-C33 \\sim O5-C32
 with sigma of 0.04
 C33-C31 \\sim C34-C32
 with sigma of 0.04
3. Rigid bond restraints
 C21, C22, C23, C24, C19, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O5 \\sim C31 \\sim C32 \\sim C33 \\sim C34: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C19 \\sim C20: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 O5, C31, C32, C33, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C14, C15, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Free rotating group:
 O5(C31,C32,C33,C34)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C17(H17A,H17B), C18(H18A,H18B), C31(H31A,H31B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 620 electrons were 
found in a volume of 3816\%A^3 in 1 void. 
This is consistent with the presence of 
4[C4H8O] per formula unit 
which account for 640.0 electrons.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              76949
_shelx_fab_checksum              70728
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 'The crystal was mounted on a None'
_olex2_submission_special_instructions 'No special instructions were received'