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_7127112
_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         'C34 H18 N4, 2 C H4 O'
_chemical_formula_sum            'C36 H26 N4 O2'
_chemical_formula_weight         546.61
_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             2019-02-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-03 deposited with the CCDC.	2020-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                84.216(4)
_cell_angle_beta                 84.817(4)
_cell_angle_gamma                79.331(4)
_cell_formula_units_Z            1
_cell_length_a                   3.7895(2)
_cell_length_b                   10.0133(5)
_cell_length_c                   18.8245(9)
_cell_measurement_reflns_used    4731
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.7030
_cell_measurement_theta_min      4.5000
_cell_volume                     696.50(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -127.00 -34.00   1.00   15.00    --  -41.67 178.00 -90.00   93
  2  \w   -112.00 -65.00   1.00   15.00    --  -41.67-137.00 -51.00   47
  3  \w    -68.00  28.00   1.00   15.00    --  -41.67  57.00 -60.00   96
  4  \w   -112.00 -15.00   1.00   15.00    --  -41.67 -57.00 150.00   97
  5  \w     39.00 118.00   1.00   30.00    --  111.00-125.00 -90.00   79
  6  \w     31.00 156.00   1.00   30.00    --  111.00 -15.00-150.00  125
  7  \w     40.00 135.00   1.00   30.00    --  111.00 -45.00  30.00   95
  8  \w     30.00 110.00   1.00   30.00    --  111.00 -94.00 -60.00   80
  9  \w     40.00 135.00   1.00   30.00    --  111.00 -45.00-150.00   95
 10  \w     40.00 135.00   1.00   30.00    --  111.00 -45.00 120.00   95
 11  \w     40.00 135.00   1.00   30.00    --  111.00 -45.00 -60.00   95
 12  \w     94.00 178.00   1.00   30.00    --  111.00 125.00 -30.00   84
 13  \w     39.00 118.00   1.00   30.00    --  111.00-125.00 -60.00   79
 14  \w     30.00 110.00   1.00   30.00    --  111.00 -94.00 -30.00   80
 15  \w     30.00 110.00   1.00   30.00    --  111.00 -94.00  60.00   80
 16  \w     66.00 178.00   1.00   30.00    --  111.00  15.00 150.00  112
 17  \w     94.00 178.00   1.00   30.00    --  111.00 125.00 120.00   84
 18  \w     39.00 118.00   1.00   30.00    --  111.00-125.00-180.00   79
 19  \w     30.00 110.00   1.00   30.00    --  111.00 -94.00-180.00   80
 20  \w     94.00 178.00   1.00   30.00    --  111.00 125.00  30.00   84
 21  \w     39.00 118.00   1.00   30.00    --  111.00-125.00  60.00   79
 22  \w     87.00 178.00   1.00   30.00    --  111.00  30.00-150.00   91
 23  \w     40.00 124.00   1.00   30.00    --  111.00-133.00  72.97   84
 24  \w   -112.00 -15.00   1.00   15.00    --  -41.67 -57.00-120.00   97
 25  \w   -112.00 -15.00   1.00   15.00    --  -41.67 -57.00  30.00   97
 26  \w   -112.00 -15.00   1.00   15.00    --  -41.67 -57.00 -30.00   97
 27  \w     57.00 128.00   1.00   15.00    --   41.67 178.00 -90.00   71
 28  \w     89.00 162.00   1.00   30.00    --  111.00  35.00  45.48   73
 29  \w     66.00 178.00   1.00   30.00    --  111.00  15.00 -30.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0749694000
_diffrn_orient_matrix_UB_12      0.0583979000
_diffrn_orient_matrix_UB_13      -0.0776472000
_diffrn_orient_matrix_UB_21      0.1347306000
_diffrn_orient_matrix_UB_22      0.1197386000
_diffrn_orient_matrix_UB_23      0.0277928000
_diffrn_orient_matrix_UB_31      0.3850815000
_diffrn_orient_matrix_UB_32      -0.0833350000
_diffrn_orient_matrix_UB_33      -0.0011206000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11081
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.227
_diffrn_reflns_theta_min         4.510
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       needle
_exptl_crystal_F_000             286
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of dichloromethane and methanol  by slow evaporation'
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2887
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0808
_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^)+(0.1466P)^2^+0.2512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2270
_refine_ls_wR_factor_ref         0.2339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2535
_reflns_number_total             2887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05311b2.cif
_cod_data_source_block           L
_cod_depositor_comments
'Adding full bibliography for 7127112--7127114.cif.'
_cod_database_code               7127112
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 Cu N5 O5'
_chemical_oxdiff_usercomment     '@ 120 K MC-Exp132'
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.764
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9182(16)
 0.0818(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C12-C13 \\sim C12-C13A
 with sigma of 0.02
 C13-C14 \\sim C13A-C14A
 with sigma of 0.02
 C13-C17 \\sim C13A-C17A
 with sigma of 0.02
 C14-N2 \\sim C14A-N2A
 with sigma of 0.02
 N2-C15 \\sim N2A-C15A
 with sigma of 0.02
 C17-C16 \\sim C17A-C16A
 with sigma of 0.02
 C15-C16 \\sim C15A-C16A
 with sigma of 0.02
 C12-C14 \\sim C12-C14A
 with sigma of 0.04
 C12-C17 \\sim C12-C17A
 with sigma of 0.04
 C13-N2 \\sim C13A-N2A
 with sigma of 0.04
 C13-C16 \\sim C13A-C16A
 with sigma of 0.04
 C14-C17 \\sim C14A-C17A
 with sigma of 0.04
 C14-C15 \\sim C14A-C15A
 with sigma of 0.04
 N2-C16 \\sim N2A-C16A
 with sigma of 0.04
 C17-C15 \\sim C17A-C15A
 with sigma of 0.04
4. Rigid body (RIGU) restrains
 N2, C13, C14, C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2A, C13A, C14A, C15A, C16A, C17A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N2A)=Sof(C13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=
 Sof(H16A)=Sof(C17A)=Sof(H17A)=1-FVAR(1)
 Sof(N2)=Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=
 Sof(C17)=Sof(H17)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C16(H16),
 C17(H17), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A)
;
_shelx_res_checksum              55255
_shelx_hkl_checksum              44898
_shelx_fab_checksum              4180
_olex2_date_sample_data_collection 2019-02-05
_olex2_date_sample_submission    2019-01-29
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id MC-Exp132
_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 1.395
_oxdiff_exptl_absorpt_empirical_full_min 0.602