Kinetic selection of Pd<sub>4</sub>L<sub>2</sub> metallocyclic and Pd<sub>6</sub>L<sub>3</sub> trigonal prismatic assemblies.
O'Connor, Helen M; Coletta, Marco; Etcheverry-Berríos, Alvaro; Nichol, Gary S.; Brechin, Euan K.; Lusby, Paul J.; Chemical communications (Cambridge, England) 56 (2020) 11799–11802; doi:10.1039/d0cc05311b

data_7127113
_publ_section_title
;
 Kinetic selection of Pd<sub>4</sub>L<sub>2</sub> metallocyclic and
 Pd<sub>6</sub>L<sub>3</sub> trigonal prismatic assemblies.
;
_journal_issue                   79
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11799
_journal_page_last               11802
_journal_paper_doi               10.1039/d0cc05311b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'C46 H50 N8 Pd2, 4(C F3 O3 S), H2 O, C4 H10 O, 1[C4H10O]'
_chemical_formula_sum            'C116 H144 F24 N16 O30 Pd4 S8'
_chemical_formula_weight         3380.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-03
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-03 deposited with the CCDC.	2020-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.016(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2080(11)
_cell_length_b                   21.440(2)
_cell_length_c                   29.333(3)
_cell_measurement_reflns_used    4225
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      21.93
_cell_measurement_theta_min      2.28
_cell_volume                     7038.9(12)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            PILATUS_2M_S_N_24_0107_Diamond
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Diamond Light Source I-19 EH1'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            99311
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.503
_diffrn_reflns_theta_min         1.141
_diffrn_source                   Synchrotron
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.348
_exptl_absorpt_correction_T_max  0.4304
_exptl_absorpt_correction_T_min  0.3060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1709 before and 0.0722 after correction.
The Ratio of minimum to maximum transmission is 0.7110.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.190
_exptl_crystal_description       needle
_exptl_crystal_F_000             6880
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of diethyl ether and nitromethane  by vapour diffusion'
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.728
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1080
_refine_ls_number_reflns         14371
_refine_ls_number_restraints     918
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0664
_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^)+(0.1533P)^2^+0.3777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2143
_refine_ls_wR_factor_ref         0.2287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10866
_reflns_number_total             14371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05311b2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7127112--7127114.cif.'
_cod_original_cell_volume        7039.0(12)
_cod_database_code               7127113
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.598
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C51-F52 = C51-F53 = C51-F51
 1.33 with sigma of 0.02
 C51-S51
 1.82 with sigma of 0.02
 S51-O51 = S51-O53 = S51-O52
 1.44 with sigma of 0.02
 C61-S61
 1.82 with sigma of 0.02
 S61-O61 = S61-O63 = S61-O62
 1.44 with sigma of 0.02
 C61-F61 = C61-F63 = C61-F62
 1.33 with sigma of 0.02
 S71-O72 = S71-O71 = S71-O73
 1.44 with sigma of 0.02
 C71-S71
 1.82 with sigma of 0.02
 C71-F73 = C71-F72 = C71-F71
 1.33 with sigma of 0.02
 C81-S81
 1.82 with sigma of 0.02
 S81A-O81A = S81A-O82A = S81A-O83A
 1.44 with sigma of 0.02
 C81-F83 = C81-F82 = C81-F81
 1.33 with sigma of 0.02
 C81A-S81A
 1.82 with sigma of 0.02
 S81-O85 = S81-O82 = S81-O81
 1.44 with sigma of 0.02
 C81A-F82A = C81A-F83A = C81A-F81A
 1.33 with sigma of 0.02
 C104-C103
 1.48 with sigma of 0.02
 C101-C102
 1.5 with sigma of 0.02
 O101-C103
 1.41 with sigma of 0.02
 O101-C101
 1.42 with sigma of 0.02
 C71A-F73A = C71A-F72A = C71A-F71A
 1.33 with sigma of 0.02
 C71A-S71A
 1.82 with sigma of 0.02
 S71A-O73A = S71A-O72A = S71A-O71A
 1.44 with sigma of 0.02
 C61A-F61A = C61A-F62A = C61A-F63A
 1.33 with sigma of 0.02
 C61A-S61A
 1.82 with sigma of 0.02
 S61A-O61A = S61A-O62A = S61A-O63A
 1.44 with sigma of 0.02
 O91-H91B = O91-H91A
 0.84 with sigma of 0.02
 C51-O53
 2.56 with sigma of 0.04
 C51-O51
 2.58 with sigma of 0.04
 C51-O52
 2.57 with sigma of 0.04
 C61-O62
 2.57 with sigma of 0.04
 C61-O61
 2.58 with sigma of 0.04
 C61-O63
 2.56 with sigma of 0.04
 C71-O71
 2.56 with sigma of 0.04
 C71-O73
 2.57 with sigma of 0.04
 C71-O72
 2.58 with sigma of 0.04
 C81A-O83A
 2.57 with sigma of 0.04
 C81A-O81A
 2.58 with sigma of 0.04
 C81-O85
 2.58 with sigma of 0.04
 C81-O81
 2.57 with sigma of 0.04
 C81A-O82A
 2.56 with sigma of 0.04
 C81-O82
 2.56 with sigma of 0.04
 O101-C104 = O101-C102
 2.37 with sigma of 0.04
 C71A-O73A
 2.58 with sigma of 0.04
 C71A-O71A
 2.57 with sigma of 0.04
 C71A-O72A
 2.56 with sigma of 0.04
 C61A-O63A
 2.57 with sigma of 0.04
 C61A-O61A
 2.58 with sigma of 0.04
 C61A-O62A
 2.56 with sigma of 0.04
 H91A-H91B
 1.35 with sigma of 0.04
 O51-O53 \\sim O53-O52 \\sim O51-O52
 with sigma of 0.04
 C51-O51 \\sim C51-O53 \\sim C51-O52
 with sigma of 0.04
 C51-F52 \\sim C51-F53 \\sim C51-F51
 with sigma of 0.02
 F52-F53 \\sim F53-F51 \\sim F51-F52
 with sigma of 0.04
 S51-F52 \\sim S51-F53 \\sim S51-F51
 with sigma of 0.04
 S51-O51 \\sim S51-O53 \\sim S51-O52
 with sigma of 0.02
 C61-F61 \\sim C61-F63 \\sim C61-F62
 with sigma of 0.02
 F61-F63 \\sim F63-F62 \\sim F62-F61
 with sigma of 0.04
 S61-F61 \\sim S61-F63 \\sim S61-F62
 with sigma of 0.04
 S61-O61 \\sim S61-O63 \\sim S61-O62
 with sigma of 0.02
 O61-O63 \\sim O63-O62 \\sim O61-O62
 with sigma of 0.04
 C61-O61 \\sim C61-O63 \\sim C61-O62
 with sigma of 0.04
 S71-O72 \\sim S71-O71 \\sim S71-O73
 with sigma of 0.02
 O72-O71 \\sim O71-O73 \\sim O72-O73
 with sigma of 0.04
 F73-F72 \\sim F72-F71 \\sim F71-F73
 with sigma of 0.04
 S71-F73 \\sim S71-F72 \\sim S71-F71
 with sigma of 0.04
 C71-F73 \\sim C71-F72 \\sim C71-F71
 with sigma of 0.02
 C71-O72 \\sim C71-O71 \\sim C71-O73
 with sigma of 0.04
 O85-O82 \\sim O82-O81 \\sim O85-O81
 with sigma of 0.04
 S81A-F82A \\sim S81A-F83A \\sim S81A-F81A
 with sigma of 0.04
 S81A-O81A \\sim S81A-O82A \\sim S81A-O83A
 with sigma of 0.02
 C81-F83 \\sim C81-F82 \\sim C81-F81
 with sigma of 0.02
 O81A-O82A \\sim O82A-O83A \\sim O81A-O83A
 with sigma of 0.04
 C81A-O81A \\sim C81A-O82A \\sim C81A-O83A
 with sigma of 0.04
 F83-F82 \\sim F82-F81 \\sim F81-F83
 with sigma of 0.04
 S81-F83 \\sim S81-F82 \\sim S81-F81
 with sigma of 0.04
 S81-O85 \\sim S81-O82 \\sim S81-O81
 with sigma of 0.02
 C81A-F82A \\sim C81A-F83A \\sim C81A-F81A
 with sigma of 0.02
 F82A-F83A \\sim F83A-F81A \\sim F81A-F82A
 with sigma of 0.04
 C81-O85 \\sim C81-O82 \\sim C81-O81
 with sigma of 0.04
 C104-C103 \\sim C101-C102
 with sigma of 0.02
 O101-C103 \\sim O101-C101
 with sigma of 0.02
 C104-O101 \\sim O101-C102
 with sigma of 0.04
 F73A-F72A \\sim F72A-F71A \\sim F71A-F73A
 with sigma of 0.04
 O73A-O72A \\sim O72A-O71A \\sim O73A-O71A
 with sigma of 0.04
 S71A-F73A \\sim S71A-F72A \\sim S71A-F71A
 with sigma of 0.04
 S71A-O73A \\sim S71A-O72A \\sim S71A-O71A
 with sigma of 0.02
 C71A-O73A \\sim C71A-O72A \\sim C71A-O71A
 with sigma of 0.04
 C71A-F73A \\sim C71A-F72A \\sim C71A-F71A
 with sigma of 0.02
 S61A-O61A \\sim S61A-O62A \\sim S61A-O63A
 with sigma of 0.02
 O61A-O62A \\sim O62A-O63A \\sim O61A-O63A
 with sigma of 0.04
 F61A-F62A \\sim F62A-F63A \\sim F63A-F61A
 with sigma of 0.04
 S61A-F61A \\sim S61A-F62A \\sim S61A-F63A
 with sigma of 0.04
 C61A-O61A \\sim C61A-O62A \\sim C61A-O63A
 with sigma of 0.04
 C61A-F61A \\sim C61A-F62A \\sim C61A-F63A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S51 \\sim F51 \\sim F52 \\sim F53 \\sim O51 \\sim O52 \\sim O53 \\sim C51:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
S61 \\sim F61 \\sim F62 \\sim F63 \\sim O61 \\sim O62 \\sim O63 \\sim C61:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
S71 \\sim F71 \\sim F72 \\sim F73 \\sim O71 \\sim O72 \\sim O73 \\sim C71:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
S81 \\sim F81 \\sim F82 \\sim F83 \\sim O81 \\sim O82 \\sim O85 \\sim C81:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
S81A \\sim F81A \\sim F82A \\sim F83A \\sim O81A \\sim O82A \\sim O83A \\sim
C81A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
O101 \\sim C101 \\sim C102 \\sim C103 \\sim C104: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
S71A \\sim F71A \\sim F72A \\sim F73A \\sim O71A \\sim O72A \\sim O73A \\sim
C71A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
S61A \\sim F61A \\sim F62A \\sim F63A \\sim O61A \\sim O62A \\sim O63A \\sim
C61A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
4. Rigid body (RIGU) restrains
 S51, F51, F52, F53, O51, O52, O53, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S71, F71, F72, F73, O71, O72, O73, C71
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S71A, F71A, F72A, F73A, O71A, O72A, O73A, C71A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S81A, F81A, F82A, F83A, O81A, O82A, O83A, C81A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S81, F81, F82, F83, O81, O82, O85, C81
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S61A, F61A, F62A, F63A, O61A, O62A, O63A, C61A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S61, F61, F62, F63, O61, O62, O63, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O101, C101, C102, C103, C104
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S81A)=Sof(F81A)=Sof(F82A)=Sof(F83A)=Sof(O81A)=Sof(O82A)=Sof(O83A)=
 Sof(C81A)=1-FVAR(1)
 Sof(S81)=Sof(F81)=Sof(F82)=Sof(F83)=Sof(O81)=Sof(O82)=Sof(O85)=Sof(C81)=FVAR(1)
 Sof(S71A)=Sof(F71A)=Sof(F72A)=Sof(F73A)=Sof(O71A)=Sof(O72A)=Sof(O73A)=
 Sof(C71A)=1-FVAR(2)
 Sof(S71)=Sof(F71)=Sof(F72)=Sof(F73)=Sof(O71)=Sof(O72)=Sof(O73)=Sof(C71)=FVAR(2)
 Sof(S61A)=Sof(F61A)=Sof(F62A)=Sof(F63A)=Sof(O61A)=Sof(O62A)=Sof(O63A)=
 Sof(C61A)=1-FVAR(3)
 Sof(S61)=Sof(F61)=Sof(F62)=Sof(F63)=Sof(O61)=Sof(O62)=Sof(O63)=Sof(C61)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C7(H7A,H7B), C8(H8A,H8B), C101(H10D,H10E),
 C103(H10I,H10J)
6.b Me refined with riding coordinates:
 C102(H10F,H10G,H10H), C104(H10K,H10L,H10M)
6.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C17(H17), C21(H21), C26(H26), C27(H27),
 C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C38(H38), C43(H43),
  C44(H44), C45(H45), C46(H46)
6.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30135
_shelx_hkl_checksum              52265
_shelx_fab_checksum              538
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id hoc1417
_olex2_submission_special_instructions 'No special instructions were received'