Homo- and and heterometallic chiral dynamic architectures from allyl-palladium(II) building blocks
Ferrer, Montserrat; Gallen, Albert; Martínez, Manuel; Rocamora, Mercè; Puttreddy, Rakesh; Rissanen, Kari; Dalton Transactions  (2022) –; doi:10.1039/D1DT03706D

data_7709772
_publ_section_title
;
 Homo- and and heterometallic chiral dynamic architectures from
 allyl-palladium(II) building blocks
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03706D
_journal_year                    2022
_chemical_formula_moiety         'C138 H134 N4 O4 P8 Pd2 Pt2, 6(C F3 O3 S)'
_chemical_formula_sum            'C144 H134 F18 N4 O22 P8 Pd2 Pt2 S6'
_chemical_formula_weight         3657.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-05-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-10-31 deposited with the CCDC.	2022-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   34.1344(8)
_cell_length_b                   39.0265(9)
_cell_length_c                   54.2199(15)
_cell_measurement_reflns_used    18761
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.0370
_cell_measurement_theta_min      3.4240
_cell_volume                     72229(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -49.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   37.0000 -180.0000 82

  2 omega -121.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  -19.0000  150.0000 121

  3 omega   23.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3676 -125.0000   90.0000 74

  4 omega   80.00  178.00   1.0000  175.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   45.0000 -120.0000 98

  5 omega   29.00   91.00   1.0000  175.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -30.0000  120.0000 62

  6 omega   77.00  178.00   1.0000  175.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   61.0000   90.0000 101

  7 omega   29.00  138.00   1.0000  175.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -77.0000  -60.0000 109

  8 omega   29.00   91.00   1.0000  175.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -30.0000  -30.0000 62

  9 omega -118.00   -9.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  -77.0000   60.0000 109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0275355000
_diffrn_orient_matrix_UB_12      -0.0235014000
_diffrn_orient_matrix_UB_13      0.0148922000
_diffrn_orient_matrix_UB_21      -0.0246366000
_diffrn_orient_matrix_UB_22      -0.0065872000
_diffrn_orient_matrix_UB_23      -0.0233771000
_diffrn_orient_matrix_UB_31      0.0259619000
_diffrn_orient_matrix_UB_32      -0.0309963000
_diffrn_orient_matrix_UB_33      -0.0062827000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0973
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            78441
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.749
_diffrn_reflns_theta_max         66.749
_diffrn_reflns_theta_min         2.989
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.367
_exptl_absorpt_correction_T_max  0.728
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       plate
_exptl_crystal_F_000             29248
_exptl_crystal_size_max          0.1734
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.0778
_refine_diff_density_max         5.434
_refine_diff_density_min         -1.872
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.602
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         15943
_refine_ls_number_restraints     259
_refine_ls_restrained_S_all      1.608
_refine_ls_R_factor_all          0.1818
_refine_ls_R_factor_gt           0.1537
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4237
_refine_ls_wR_factor_ref         0.4682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9448
_reflns_number_total             15943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03706d2.cif
_cod_data_source_block           1PtaL_2
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7709772
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H25 N4 P1 S1 F3 O3 Pd1'
_shelx_estimated_absorpt_t_max   0.637
_shelx_estimated_absorpt_t_min   0.405
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 F6-C71
 1.2 with sigma of 0.02
 C71-F5
 1.2 with sigma of 0.02
 F5-S3
 2.4 with sigma of 0.02
 C71-F4
 1.2 with sigma of 0.02
 F4-S3
 2.4 with sigma of 0.02
 C70-F2
 1.2 with sigma of 0.02
 C70-F1
 1.2 with sigma of 0.02
 C70-F3
 1.2 with sigma of 0.02
 C73-F12
 1.3 with sigma of 0.02
 C73-S2
 2.1 with sigma of 0.02
 S2-F12
 2.5 with sigma of 0.02
 F10-C73
 1.3 with sigma of 0.02
 S2-F10
 2.5 with sigma of 0.02
 F12-F10
 2.1 with sigma of 0.02
 S4-O10
 1.46 with sigma of 0.02
 C72-S4
 1.8 with sigma of 0.02
 S2-O8
 1.4 with sigma of 0.02
 F12-O8
 2.8 with sigma of 0.02
 O9-O8
 2.5 with sigma of 0.02
 F9-C72
 1.3 with sigma of 0.02
 F8-C72
 1.3 with sigma of 0.02
 C72-F7
 1.3 with sigma of 0.02
 F9-F7
 2.1 with sigma of 0.02
 F12-F11
 2.1 with sigma of 0.02
 F11-F10
 2.1 with sigma of 0.02
 F11-S2
 2.5 with sigma of 0.02
 C67-C68
 1.5 with sigma of 0.02
 C68-O2
 1.5 with sigma of 0.02
 C65-C64
 1.5 with sigma of 0.02
 O2-C65
 1.4 with sigma of 0.02
 C31-C33
 1.51 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C56) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C42)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C68) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C60) \\sim Ueq, Uanis(C57) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C64) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C73) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(F12) \\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(F10) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(S2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O10) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(F10) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(O11) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C72) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F9) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F11) \\sim
Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(F11) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O2) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C49) \\sim Ueq,
Uanis(C48) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C69) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(S1) = Uanis(C70)
Uanis(F2) = Uanis(F1)
Uanis(C51) = Uanis(C54)
Uanis(O6) = Uanis(O5)
Uanis(F5) = Uanis(F6)
Uanis(C21) = Uanis(C18)
Uanis(F3) = Uanis(F1)
Uanis(C71) = Uanis(S3)
Uanis(C45) = Uanis(C48)
Uanis(C50) = Uanis(C46)
Uanis(F6) = Uanis(F4) = Uanis(F5)
Uanis(C72) = Uanis(S4)
Uanis(C72) = Uanis(F9)
Uanis(C72) = Uanis(F8)
Uanis(C72) = Uanis(F7)
Uanis(C64) = Uanis(C67)
Uanis(C69) = Uanis(C65)
Uanis(F5) = Uanis(F6) = Uanis(F4) = Uanis(C71)
4. Others
 Fixed Sof: S1(0.5) S2(0.5) F1(0.5) F2(0.5) F3(0.5) F10(0.5) F11(0.5) F12(0.5)
 O3(0.5) O8(0.5) C70(0.5) C73(0.5)
 Fixed U11: S4(0.21232) F7(0.21232) F8(0.21232) F9(0.21232) F11(0.13351)
 O8(0.14193) O10(0.27643) O11(0.21823) C65(0.26087) C69(0.26087) C72(0.21232)
5.a Riding coordinates:
 C67(H67A,H67B,H67C), C69(H69A,H69B,H69C)
5.b Ternary CH refined with riding coordinates:
 C64(H64), C65(H65)
5.c Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C32(H32A,H32B), C63(H63A,H63B), C66(H66A,H66B)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C2(H2), C1(H1), C34(H34), C35(H35), C37(H37), C38(H38),
 C11(H11), C10(H10), C9(H9), C8(H8), C7(H7), C15(H15), C14(H14), C13(H13),
 C17(H17), C16(H16), C21(H21), C20(H20), C19(H19), C23(H23), C22(H22), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C44(H44), C43(H43), C42(H42),
 C41(H41), C40(H40), C50(H50), C49(H49), C48(H48), C47(H47), C46(H46), C56(H56),
  C55(H55), C54(H54), C53(H53), C52(H52), C58(H58), C59(H59), C60(H60),
 C61(H61), C62(H62)
5.e Fitted hexagon refined as free rotating group:
 N1(C5,C4,C3,C2,C1), N2(C34,C35,C36,C37,C38), C6(C11,C10,C9,C8,C7), C15(C14,
 C13,C12,C17,C16), C21(C20,C19,C18,C23,C22), C25(C26,C27,C28,C29,C24), C39(C44,
 C43,C42,C41,C40), C45(C50,C49,C48,C47,C46), C51(C56,C55,C54,C53,C52), C57(C58,
 C59,C60,C61,C62)
5.f Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'