A symmetry interaction approach to [M2L2]4+ metallocycles and their self-catenation
Preston, Dan; Inglis, Amanda R.; Garden, Anna L.; Kruger, Paul; Chemical Communications  (2019) –; doi:10.1039/C9CC07130J

data_7124290
_publ_section_title
;
 A symmetry interaction approach to [M2L2]4+ metallocycles and their
 self-catenation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07130J
_journal_year                    2019
_chemical_formula_moiety         'C42 H30 N14 Pd2, 4(B F4), 6(C3 H7 N O)'
_chemical_formula_sum            'C60 H72 B4 F16 N20 O6 Pd2'
_chemical_formula_weight         1729.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-06 deposited with the CCDC.    2019-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                95.966(2)
_cell_angle_beta                 90.358(2)
_cell_angle_gamma                111.455(3)
_cell_formula_units_Z            1
_cell_length_a                   8.7458(3)
_cell_length_b                   9.9923(3)
_cell_length_c                   22.1097(6)
_cell_measurement_reflns_used    10420
_cell_measurement_temperature    119.98(11)
_cell_measurement_theta_max      72.5390
_cell_measurement_theta_min      3.9870
_cell_volume                     1786.50(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (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      119.98(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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    -62.00 -13.00   1.00    3.00    --  -38.50 -57.00  60.00   49
  2  \w   -107.00 -65.00   1.00    3.00    --  -38.50 -57.00  60.00   42
  3  \w   -103.00 -67.00   1.00    3.00    --  -38.50 -57.00 150.00   36
  4  \w    -84.00  -2.00   1.00    3.00    --  -38.50 125.00  90.00   82
  5  \w    -99.00 -13.00   1.00    3.00    --  -38.50 -57.00 -60.00   86
  6  \w    -54.00 -13.00   1.00    3.00    --  -38.50 -57.00 150.00   41
  7  \w    -89.00  -2.00   1.00    3.00    --  -38.50 125.00 -90.00   87
  8  \w      7.00  32.00   1.00    3.00    --   42.00  89.00-109.51   25
  9  \w     10.00  35.00   1.00    3.00    --   42.00  84.00  -6.72   25
 10  \w     16.00  41.00   1.00    3.00    --   46.00  81.00 160.56   25
 11  \w     19.00  44.00   1.00    3.00    --   50.00  81.00  32.29   25
 12  \w     19.00  44.00   1.00    3.00    --   50.00  81.00  57.91   25
 13  \w     19.00  44.00   1.00    3.00    --   50.00  81.00-137.88   25
 14  \w     26.00  53.00   1.00    3.00    --   54.00  75.00 -60.04   27
 15  \w     29.00  56.00   1.00    3.00    --   58.00  74.00 118.45   27
 16  \w     30.00  59.00   1.00    3.00    --   58.00  77.00 -32.51   29
 17  \w     32.00  64.00   1.00    3.00    --   62.00  77.00-110.31   32
 18  \w     32.00  59.00   1.00    3.00    --   62.00  77.00 148.24   27
 19  \w     36.00  62.00   1.00    3.00    --   66.00  75.00 177.26   26
 20  \w     37.00  80.00   1.00    3.00    --   66.00  76.00  16.90   43
 21  \w     98.00 125.00   1.00    3.00    --   66.00  75.00 177.26   27
 22  \w     41.00  68.00   1.00    3.00    --   70.00  73.00 -18.12   27
 23  \w     91.00 134.00   1.00    3.00    --   70.00  75.00-156.20   43
 24  \w     42.00  74.00   1.00    3.00    --   70.00  75.00-156.20   32
 25  \w     41.00  66.00   1.00    3.00    --   70.00  76.00 -79.12   25
 26  \w     41.00  68.00   1.00    3.00    --   70.00  75.00  67.27   27
 27  \w     49.00  74.00   1.00   12.00    --   74.00  61.00 -81.52   25
 28  \w     48.00  96.00   1.00   12.00    --   74.00  64.00 157.37   48
 29  \w     51.00 131.00   1.00   12.00    --   78.00  66.00  45.88   80
 30  \w     52.00  86.00   1.00   12.00    --   82.00  76.00  83.86   34
 31  \w     62.00  89.00   1.00   12.00    --   82.00  70.00-127.57   27
 32  \w     55.00  82.00   1.00   12.00    --   82.00  66.00 -21.82   27
 33  \w     61.00  93.00   1.00   12.00    --   86.00  69.00 107.43   32
 34  \w     61.00  89.00   1.00   12.00    --   90.00  71.00 -73.53   28
 35  \w     65.00  96.00   1.00   12.00    --   94.00  72.00-164.64   31
 36  \w     68.00 150.00   1.00   12.00    --   94.00  63.00 -47.58   82
 37  \w    118.00 163.00   1.00   12.00    --   94.00  70.00 -22.10   45
 38  \w     66.00  92.00   1.00   12.00    --   94.00  70.00 -22.10   26
 39  \w     99.00 164.00   1.00   12.00    --   94.00  72.00-164.64   65
 40  \w     73.00 128.00   1.00   12.00    --   98.00  57.00-162.24   55
 41  \w     77.00 171.00   1.00   12.00    --  102.86  61.00  30.00   94
 42  \w     80.00 107.00   1.00   12.00    --  102.86  45.00  30.00   27
 43  \w     52.00 104.00   1.00   12.00    --  102.86 -94.00  30.00   52
 44  \w    144.00 171.00   1.00   12.00    --  102.86  77.00 -30.00   27
 45  \w     73.00 150.00   1.00   12.00    --  102.86  77.00-120.00   77
 46  \w     46.00 128.00   1.00   12.00    --  102.86 -61.00-180.00   82
 47  \w     73.00 156.00   1.00   12.00    --  102.86  77.00  60.00   83
 48  \w     30.00  96.00   1.00   12.00    --  102.86 -94.00 120.00   66
 49  \w    105.00 172.00   1.00   12.00    --  102.86  77.00 -90.00   67
 50  \w     77.00 104.00   1.00   12.00    --  102.86  77.00 -90.00   27
 51  \w     39.00  93.00   1.00   12.00    --  102.86-125.00  30.00   54
 52  \w     75.00 107.00   1.00   12.00    --  102.86  77.00 -30.00   32
 53  \w     73.00 148.00   1.00   12.00    --  102.86  77.00 120.00   75
 54  \w    105.00 174.00   1.00   12.00    --  102.86  77.00 150.00   69
 55  \w     73.00  99.00   1.00   12.00    --  102.86  77.00 150.00   26
 56  \w     79.00 118.00   1.00   12.00    --  102.86-125.00 -30.00   39
 57  \w    140.00 174.00   1.00   12.00    --  102.86  77.00-150.00   34
 58  \w     77.00 111.00   1.00   12.00    --  102.86  77.00-150.00   34
 59  \w     76.00 174.00   1.00   12.00    --  102.86  77.00  90.00   98
 60  \w     28.00 103.00   1.00   12.00    --  102.86 -94.00-180.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0359352000
_diffrn_orient_matrix_UB_12      -0.0860356000
_diffrn_orient_matrix_UB_13      0.0555562000
_diffrn_orient_matrix_UB_21      -0.1353766000
_diffrn_orient_matrix_UB_22      -0.1262001000
_diffrn_orient_matrix_UB_23      -0.0380101000
_diffrn_orient_matrix_UB_31      0.1276100000
_diffrn_orient_matrix_UB_32      -0.0668930000
_diffrn_orient_matrix_UB_33      -0.0196987000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0997
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31571
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.886
_diffrn_reflns_theta_min         4.025
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.996
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.264
_refine_diff_density_min         -1.467
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+1.6338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5843
_reflns_number_total             6981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07130j3.cif
_cod_data_source_block           dp097c
_cod_database_code               7124290
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H30 B4 F16 N14 Pd2'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C16(H16), C7(H7), C14(H14), C21(H21), C12(H12), C5(H5), C20(H20),
 C18(H18), C19(H19), C6(H6), C2(H2), C13(H13), C3(H3), C1(H1), C27(H27),
 C28(H28), C24(H24)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C23(H23A,H23B,
 H23C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              40964
_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 1.854
_oxdiff_exptl_absorpt_empirical_full_min 0.691