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_7703256
_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
'C100 H112 Cl8 Mo2 O8 P4 Ru4, 6(C H2 Cl2), 1[CH2Cl2], 2[CH2Cl2]'
_chemical_formula_sum            'C109 H130 Cl26 Mo2 O8 P4 Ru4'
_chemical_formula_weight         3209.86
_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                91.633(7)
_cell_angle_beta                 100.343(7)
_cell_angle_gamma                102.881(6)
_cell_formula_units_Z            1
_cell_length_a                   11.4314(10)
_cell_length_b                   17.3797(13)
_cell_length_c                   17.3723(16)
_cell_measurement_reflns_used    23718
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.91
_cell_measurement_theta_min      1.64
_cell_volume                     3301.4(5)
_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 0.989
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
 247 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  0.0811
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23611
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.242
_diffrn_reflns_theta_min         1.635
_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    1.255
_exptl_absorpt_correction_T_max  0.9283
_exptl_absorpt_correction_T_min  0.8021
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRED & LANA'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       prism
_exptl_crystal_F_000             1610
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.062
_refine_diff_density_max         2.037
_refine_diff_density_min         -1.985
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         12919
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1406
_refine_ls_R_factor_gt           0.0931
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1537P)^2^+18.9643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2392
_refine_ls_wR_factor_ref         0.2821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8089
_reflns_number_total             12919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04167b2.cif
_cod_data_source_block           nkca012-1
_cod_depositor_comments
'Adding full bibliography for 7703254--7703259.cif.'
_cod_database_code               7703256
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C22, C23, C24, C21, C16, C20, C19, C17, C18, C25
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.008
3. Uiso/Uaniso restraints and constraints
C24 \\sim C23 \\sim C22 \\sim C21 \\sim C16 \\sim C20 \\sim C19 \\sim C18 \\sim
C17 \\sim C25: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4.a Ternary CH refined with riding coordinates:
 C20(H20), C22(H22), C47(H47)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C27(H27A,H27B), C28(H28A,H28B), C51(H51A,H51B),
 C52(H52A,H52B), C53(H53A,H53B)
4.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), C16(H16), C17(H17), C19(H19), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
 C41(H41), C43(H43), C44(H44), C46(H46)
4.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 121 electrons were 
found in a volume of 432\%A^3 in 2 voids. 
This is consistent with the presence of 
1[CH2Cl2], 2[CH2Cl2] per formula unit 
which account for 126.0 electrons.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              73253
_shelx_fab_checksum              74240
_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'