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_7703255
_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         'C88 H64 Au4 F20 Mo2 O9 P4, 2.5(C4 H8 O)'
_chemical_formula_sum            'C98 H84 Au4 F20 Mo2 O11.5 P4'
_chemical_formula_weight         2929.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-20
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-24 deposited with the CCDC.	2020-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                115.497(2)
_cell_angle_beta                 92.100(2)
_cell_angle_gamma                110.887(2)
_cell_formula_units_Z            2
_cell_length_a                   16.7915(4)
_cell_length_b                   18.7734(5)
_cell_length_c                   19.3826(5)
_cell_measurement_reflns_used    35031
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.86
_cell_measurement_theta_min      1.19
_cell_volume                     5019.9(3)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.127.0 (STOE, 2016)'
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area X-Red32 1.63.2.0 (STOE, 2017)
;
_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      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_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  0.0469
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42389
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.134
_diffrn_reflns_theta_min         1.195
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.224
_exptl_absorpt_correction_T_max  0.5648
_exptl_absorpt_correction_T_min  0.2262
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRED, XSHAPE & LANA'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_description       plate
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.096
_refine_diff_density_max         4.655
_refine_diff_density_min         -1.740
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1261
_refine_ls_number_reflns         19696
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0560
_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^)+(0.1101P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15347
_reflns_number_total             19696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04167b2.cif
_cod_data_source_block           nk102
_cod_depositor_comments
'Adding full bibliography for 7703254--7703259.cif.'
_cod_original_cell_volume        5019.9(2)
_cod_original_formula_sum        'C98 H84 Au4 F20 Mo2 O11.50 P4'
_cod_database_code               7703255
_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
 C97-C98 \\sim C98-C99 \\sim C99-C100
 with sigma of 0.02
 O12-C97 \\sim O12-C100
 with sigma of 0.02
 O12-C98 \\sim O12-C99
 with sigma of 0.04
 C98-C100 \\sim C97-C99
 with sigma of 0.04
 C89-C90 \\sim C90-C91 \\sim C91-C92
 with sigma of 0.02
 O10-C89 \\sim O10-C92
 with sigma of 0.02
 O10-C90 \\sim O10-C91
 with sigma of 0.04
 C90-C92 \\sim C89-C91
 with sigma of 0.04
3. Rigid bond restraints
 P3, Au3, C52, C46, C53, C45, C51, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O12 \\sim C97 \\sim C98 \\sim C99 \\sim C100: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O10 \\sim C89 \\sim C90 \\sim C91 \\sim C92: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 O12, C97, C98, C99, C100
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C89, C90, C91, C92
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O12(0.5) C97(0.5) H97A(0.5) H97B(0.5) C98(0.5) H98A(0.5) H98B(0.5)
 C99(0.5) H99A(0.5) H99B(0.5) C100(0.5) H10A(0.5) H10B(0.5)
7.a Free rotating group:
 O10(C89,C90,C91,C92), O12(C97,C98,C99,C100)
7.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C23(H23A,H23B), C24(H24A,H24B), C44(H44A,H44B),
 C45(H45A,H45B), C65(H65A,H65B), C66(H66A,H66B), C85(H85A,H85B), C86(H86A,H86B),
  C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,
 H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
 C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C100(H10A,H10B)
7.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), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C47(H47), C48(H48), C49(H49),
 C50(H50), C51(H51), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C68(H68),
  C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76),
 C77(H77), C78(H78)
;
_shelx_res_checksum              60707
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop oil'
_olex2_submission_special_instructions 'No special instructions were received'