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_7709771
_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 Pd4, 6(C F3 O3 S)'
_chemical_formula_sum            'C144 H134 F18 N4 O22 P8 Pd4 S6'
_chemical_formula_weight         3480.26
_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
_audit_creation_date             2020-05-25
_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                   34.0893(10)
_cell_length_b                   39.0572(5)
_cell_length_c                   53.629(2)
_cell_measurement_reflns_used    14376
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      72.7870
_cell_measurement_theta_min      3.4260
_cell_volume                     71403(4)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega -126.00 -100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176    0.0000  150.0000 26

  2 omega  -68.00   25.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176   57.0000    0.0000 93

  3 omega  -59.00   47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1176    0.0000  150.0000 106

  4 omega  107.00  174.00   1.0000  105.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  105.0000  107.0000 67

  5 omega   94.00  174.00   1.0000  105.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  125.0000   60.0000 80

  6 omega   73.00  178.00   1.0000  105.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154   77.0000    0.0000 105

  7 omega   33.00  135.00   1.0000  105.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6154  -61.0000   60.0000 102
;
_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      0.0298449000
_diffrn_orient_matrix_UB_12      -0.0217498000
_diffrn_orient_matrix_UB_13      0.0147000000
_diffrn_orient_matrix_UB_21      -0.0253754000
_diffrn_orient_matrix_UB_22      0.0035864000
_diffrn_orient_matrix_UB_23      0.0236227000
_diffrn_orient_matrix_UB_31      -0.0225895000
_diffrn_orient_matrix_UB_32      -0.0326964000
_diffrn_orient_matrix_UB_33      -0.0071625000
_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  0.0520
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            53165
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.500
_diffrn_reflns_theta_min         3.012
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64659
_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)
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    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             28224
_exptl_crystal_size_max          0.2541
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.1434
_refine_diff_density_max         2.613
_refine_diff_density_min         -1.515
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       0.000012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.566
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         15723
_refine_ls_number_restraints     188
_refine_ls_restrained_S_all      1.580
_refine_ls_R_factor_all          0.1775
_refine_ls_R_factor_gt           0.1443
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4136
_refine_ls_wR_factor_ref         0.4559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9243
_reflns_number_total             15723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03706d2.cif
_cod_data_source_block           1PdaL_2
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7709771
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C68 H60 N2 Pd2 P1 S1 O3 F3'
_shelx_estimated_absorpt_t_max   0.524
_shelx_estimated_absorpt_t_min   0.353
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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
 C71-F6
 1.2 with sigma of 0.02
 C68-C67
 1.54 with sigma of 0.01
 F5-C71
 1.2 with sigma of 0.02
 C72-F11
 1.2 with sigma of 0.02
 C72-F10
 1.2 with sigma of 0.02
 F12-C72
 1.2 with sigma of 0.02
 O12-S3
 1.4 with sigma of 0.02
 C71-S2
 1.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O8) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F7) \\sim
Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C47) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C46)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O3) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(O1)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C40) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C48) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O5) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C16) \\sim
Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(F4) \\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F1) \\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(C70) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C67) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
Uanis(C68) = Uanis(C67)
Uanis(C57) = Uanis(C60)
Uanis(C42) = Uanis(C39)
Uanis(F4) = Uanis(F5)
Uanis(F10) = Uanis(F11)
Uanis(F10) = Uanis(C72)
Uanis(F8) = Uanis(O12)
Uanis(C71) = Uanis(S2)
Uanis(F4) = Uanis(F6) = Uanis(F5) = Uanis(C71)
Uanis(O5) = Uanis(O6) = Uanis(O4)
4. Others
 Fixed Sof: S1(0.5) S3(0.5) F1(0.5) F2(0.5) F3(0.5) F7(0.5) F8(0.5) F9(0.5)
 O7(0.5) O12(0.5) C70(0.5) C73(0.5)
5.a Riding coordinates:
 C69(H69A,H69B,H69C)
5.b Ternary CH refined with riding coordinates:
 C64(H64), C65(H65)
5.c Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C20(H20A,H20B), C63(H63A,H63B), C66(H66A,H66B)
5.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C37(H37), C38(H38), C44(H44), C40(H40), C41(H41), C42(H42),
  C43(H43), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52),
 C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61),
  C62(H62)
5.e Fitted hexagon refined as free rotating group:
 C44(C39,C40,C41,C42,C43), C45(C46,C47,C48,C49,C50)
5.f Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C68(H68A,H68B,H68C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'