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_7703257
_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
'C92 H104 Cl4 Ir4 Mo2 O8 P4, 4(C4 H8 O), 3[C4H8O]'
_chemical_formula_sum            'C120 H160 Cl4 Ir4 Mo2 O15 P4'
_chemical_formula_weight         3068.83
_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.r5530)
;
_audit_update_record
;
2019-10-24 deposited with the CCDC.	2020-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                105.261(2)
_cell_angle_beta                 102.501(2)
_cell_angle_gamma                104.496(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8365(3)
_cell_length_b                   16.7623(5)
_cell_length_c                   20.7559(6)
_cell_measurement_reflns_used    21438
_cell_measurement_temperature    210
_cell_measurement_theta_max      29.21
_cell_measurement_theta_min      1.97
_cell_volume                     3356.71(18)
_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      210
_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 0.984
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
 188 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  0.0341
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23002
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.092
_diffrn_reflns_theta_min         1.967
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           0.000
_diffrn_source_power             0.000
_diffrn_source_voltage           0
_exptl_absorpt_coefficient_mu    4.311
_exptl_absorpt_correction_T_max  0.4714
_exptl_absorpt_correction_T_min  0.2691
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRED & LANA'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       prism
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.302
_exptl_crystal_size_min          0.196
_refine_diff_density_max         1.383
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         13039
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+2.5562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10553
_reflns_number_total             13039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04167b2.cif
_cod_data_source_block           nk110
_cod_depositor_comments
'Adding full bibliography for 7703254--7703259.cif.'
_cod_original_cell_volume        3356.71(17)
_cod_database_code               7703257
_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
 C51-C52 \\sim C52-C53 \\sim C53-C54
 with sigma of 0.02
 O6-C51 \\sim O6-C54
 with sigma of 0.02
 O6-C52 \\sim O6-C53
 with sigma of 0.04
 C52-C54 \\sim C51-C53
 with sigma of 0.04
 C58-C57 \\sim C57-C56 \\sim C56-C55
 with sigma of 0.02
 O7-C58 \\sim O7-C55
 with sigma of 0.02
 O7-C57 \\sim O7-C56
 with sigma of 0.04
 C57-C55 \\sim C58-C56
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O6 \\sim C51 \\sim C52 \\sim C53 \\sim C54: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O7 \\sim C55 \\sim C56 \\sim C57 \\sim C58: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O6, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7, C55, C56, C57, C58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O6(0.5) C51(0.5) H51A(0.5) H51B(0.5) C52(0.5) H52A(0.5) H52B(0.5)
 C53(0.5) H53A(0.5) H53B(0.5) C54(0.5) H54A(0.5) H54B(0.5) O7(0.5) C55(0.5)
 H55A(0.5) H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5) C57(0.5) H57A(0.5) H57B(0.5)
 C58(0.5) H58A(0.5) H58B(0.5)
6.a Free rotating group:
 O6(C51,C52,C53,C54), O7(C55,C56,C57,C58)
6.b Ternary CH refined with riding coordinates:
 C16(H16), C17(H17), C20(H20), C21(H21), C39(H39), C40(H40), C43(H43), C44(H44)
6.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C18(H18A,H18B), C19(H19A,H19B), C22(H22A,H22B),
 C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C41(H41A,H41B), C42(H42A,H42B),
  C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,
 H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
 C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B)
6.d 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), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34),
  C35(H35), C36(H36), C37(H37), C38(H38)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 102 electrons were 
found in a volume of 646\%A^3 in 2 voids. 
This is consistent with the presence of 
3[C4H8O] per formula unit 
which account for 120.0 electrons.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90884
_shelx_fab_checksum              61996
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_submission_special_instructions 'No special instructions were received'