"Bottled" spiro-doubly aromatic trinuclear [Pd<sub>2</sub>Ru]<sup>+</sup> complexes.
Kulichenko, Maksim; Fedik, Nikita; Monfredini, Anna; Muñoz-Castro, Alvaro; Balestri, Davide; Boldyrev, Alexander I.; Maestri, Giovanni; Chemical science 12 (2020) 477–486; doi:10.1039/d0sc04469e

data_1559999
_publ_section_title
;
 "Bottled" spiro-doubly aromatic trinuclear [Pd<sub>2</sub>Ru]<sup>+</sup>
 complexes.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              477
_journal_page_last               486
_journal_paper_doi               10.1039/d0sc04469e
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety
'C64 H59 P2 Pd2 Ru S3, 2(F3 Sb0.5), 0.5(C H Cl3)'
_chemical_formula_sum            'C64.5 H59.5 Cl1.5 F6 P2 Pd2 Ru S3 Sb'
_chemical_formula_weight         1595.53
_chemical_name_systematic
bis(triphenylphosphine)-tris(phenylthiolate)-bispalladium-ruthenium-hexafluoroantimoniate-dichloromethane
_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             2020-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-20 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                94.5180(16)
_cell_angle_beta                 91.0356(18)
_cell_angle_gamma                101.5240(16)
_cell_formula_units_Z            2
_cell_length_a                   11.9921(3)
_cell_length_b                   12.28439(18)
_cell_length_c                   21.7330(5)
_cell_measurement_reflns_used    32551
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.8820
_cell_measurement_theta_min      1.7060
_cell_volume                     3125.45(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS (Kabsch, 2010) -CCP4 (Evans, 2013)'
_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                 'Pilatus 2M'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       synchrotron
_diffrn_measurement_device_type
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
_diffrn_measurement_method       'Rotating Crystal'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0477778000
_diffrn_orient_matrix_UB_12      0.0167778000
_diffrn_orient_matrix_UB_13      -0.0120839000
_diffrn_orient_matrix_UB_21      0.0168634000
_diffrn_orient_matrix_UB_22      -0.0123417000
_diffrn_orient_matrix_UB_23      -0.0299851000
_diffrn_orient_matrix_UB_31      -0.0314015000
_diffrn_orient_matrix_UB_32      -0.0545189000
_diffrn_orient_matrix_UB_33      0.0001589000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            76077
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         25.264
_diffrn_reflns_theta_min         0.926
_diffrn_source                   'Elettra Synchrotron- XRD1 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1582
_exptl_crystal_preparation       'From dichloromethane solution'
_exptl_crystal_recrystallization_method
'n-hexane vapour diffusion into dichloromethane solution'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.046
_refine_diff_density_min         -1.669
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         11759
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0770P)^2^+55.3382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11699
_reflns_number_total             11759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04469e2.cif
_cod_data_source_block           am230v-bis_1_
_cod_depositor_comments          'Adding full bibliography for 1559999.cif.'
_cod_original_cell_volume        3125.45(11)
_cod_original_formula_sum        'C64.50 H59.50 Cl1.50 F6 P2 Pd2 Ru S3 Sb'
_cod_database_code               1559999
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.810
_reflns_odcompleteness_completeness 73.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.73
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Sb2-F72
 1.8 with sigma of 0.02
 Sb2-F62
 1.8 with sigma of 0.02
 Sb2-F52
 1.8 with sigma of 0.02
 F62-Sb2
 1.8 with sigma of 0.02
 Sb2-F22
 1.8 with sigma of 0.02
 F52-Sb2
 1.8 with sigma of 0.02
 F42-Sb2
 1.8 with sigma of 0.02
 Sb2-F32
 1.8 with sigma of 0.02
 F11-F3A
 2.6 with sigma of 0.04
 F62-F22
 2.6 with sigma of 0.04
 F52-F22
 2.6 with sigma of 0.04
 F22-F62
 2.6 with sigma of 0.04
 F52-F72
 2.6 with sigma of 0.04
 F62-F52
 2.6 with sigma of 0.04
 F62-F32
 2.6 with sigma of 0.04
 F72-F32
 2.6 with sigma of 0.04
 F32-F62
 2.6 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C51) = Uanis(C1S)
Uanis(F42) = Uanis(F62) = Uanis(F52) = Uanis(F32) = Uanis(F72) = Uanis(F22)
4. Others
 Sof(F2A)=Sof(F1A)=Sof(F3A)=1-FVAR(1)
 Sof(F11)=Sof(F31)=Sof(F21)=FVAR(1)
 Fixed Sof: Sb2(0.5) F52(0.5) F22(0.5) F32(0.5) F62(0.5) F72(0.5) F42(0.5)
 Cl1S(0.5) Cl3S(0.5) Cl2S(0.5) C1S(0.5) H1S(0.5)
 Fixed X: C1S(0.03852)
 Fixed Y: C1S(0.83004)
 Fixed Z: C1S(0.46616)
5.a Free rotating group:
 Cl3S(Cl2S)
5.b Ternary CH refined with riding coordinates:
 C86(H86), C1S(H1S)
5.c Aromatic/amide H refined with riding coordinates:
 C64(H64), C22(H22), C182(H182), C32(H32), C26(H26), C65(H65), C161(H161),
 C36(H36), C82(H82), C24(H24), C34(H34), C141(H141), C62(H62), C42(H42),
 C81(H81), C142(H142), C181(H181), C172(H172), C151(H151), C52(H52), C63(H63),
 C54(H54), C33(H33), C112(H112), C92(H92), C23(H23), C122(H122), C162(H162),
 C171(H171), C21(H21), C25(H25), C44(H44), C35(H35), C121(H121), C111(H111),
 C102(H102), C55(H55), C56(H56), C91(H91), C61(H61), C152(H152), C66(H66),
 C101(H101), C43(H43), C51(H51), C31(H31), C45(H45), C53(H53), C41(H41)
5.d Idealised Me refined as rotating group:
 C76(H76A,H76B,H76C), C96(H96A,H96B,H96C), C106(H10A,H10B,H10C)
;
_shelx_res_checksum              60933
_olex2_exptl_crystal_mounting_method '0.3mm Cryoloop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.672
_oxdiff_exptl_absorpt_empirical_full_min 0.744