Construction of Pd-based coordination cages with three geometrically distinct ligands.
Li, Ru-Jin; de Montmollin, Jean; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Severin, Kay; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt00248a

data_7712857
_publ_section_title
;
 Construction of Pd-based coordination cages with three geometrically
 distinct ligands.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt00248a
_journal_year                    2023
_chemical_formula_moiety         'C64 H40 N8 Pd2, 4(B F4), 6[C2H3N]'
_chemical_formula_sum            'C64 H40 B4 F16 N8 Pd2'
_chemical_formula_weight         1481.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-01-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-19 deposited with the CCDC.	2023-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.507(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3697(2)
_cell_length_b                   65.3984(8)
_cell_length_c                   11.7619(2)
_cell_measurement_reflns_used    27685
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      74.2020
_cell_measurement_theta_min      2.6810
_cell_volume                     7685.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.958
_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     32.00  71.14   0.38    5.00    --   66.10 -95.00-180.00  103
  2  \w     31.00  58.36   0.38    5.00    --   66.10 -95.00 -60.00   72
  3  \w     37.00 108.06   0.38    5.00    --   66.10  15.00-150.00  187
  4  \w     42.00  72.78   0.38    5.00    --   66.10 -95.00 -30.00   81
  5  \w   -104.00 -78.92   0.38    5.00    --  -67.15   0.00-120.00   66
  6  \w   -104.00 -77.78   0.38    5.00    --  -67.15   0.00 120.00   69
  7  \w   -101.00 -73.64   0.38    5.00    --  -67.15   0.00 150.00   72
  8  \w   -104.00 -75.12   0.38    5.00    --  -67.15   0.00 -90.00   76
  9  \w   -105.00 -73.08   0.38    5.00    --  -69.26   0.00-180.00   84
 10  \w   -107.00 -71.66   0.38    5.00    --  -69.26   0.00-120.00   93
 11  \w     34.00  80.36   0.38    5.00    --   69.47-125.00 -90.00  122
 12  \w     40.00  81.80   0.38    5.00    --   69.47  15.00  90.00  110
 13  \w     39.00  65.22   0.38    5.00    --   69.47-125.00   0.00   69
 14  \w     39.00  74.34   0.38    5.00    --   69.47 -95.00  60.00   93
 15  \w     32.00  70.00   0.38    5.00    --   69.47 -95.00 -90.00  100
 16  \w     74.00  99.08   0.38    5.00    --   69.47  15.00 120.00   66
 17  \w     40.00  73.06   0.38    5.00    --   78.01 -95.00   0.00   87
 18  \w     37.00  66.64   0.38    5.00    --   78.01-125.00-180.00   78
 19  \w     42.00  77.72   0.38    5.00    --   78.01 -95.00-150.00   94
 20  \w     51.00  84.82   0.38    5.00    --   78.01 -95.00 -60.00   89
 21  \w     64.00  97.82   0.38    5.00    --   78.01  15.00 150.00   89
 22  \w     47.00 123.00   0.38    5.00    --   78.01  15.00  90.00  200
 23  \w     54.00 117.08   0.38    5.00    --   78.01  15.00   0.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0281106000
_diffrn_orient_matrix_UB_12      -0.0100847000
_diffrn_orient_matrix_UB_13      0.1288648000
_diffrn_orient_matrix_UB_21      0.0901256000
_diffrn_orient_matrix_UB_22      0.0181649000
_diffrn_orient_matrix_UB_23      0.0747404000
_diffrn_orient_matrix_UB_31      -0.1218899000
_diffrn_orient_matrix_UB_32      0.0111128000
_diffrn_orient_matrix_UB_33      -0.0050388000
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       81
_diffrn_reflns_limit_k_min       -77
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            57817
_diffrn_reflns_point_group_measured_fraction_full 0.903
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.693
_diffrn_reflns_theta_min         2.703
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.460
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       prism
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.974
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.245(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1693
_refine_ls_number_reflns         26588
_refine_ls_number_restraints     2729
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0620
_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^)+(0.1174P)^2^+0.6828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1748
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    0.807
_reflns_Friedel_fraction_max     0.727
_reflns_number_gt                22790
_reflns_number_total             26588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00248a2.cif
_cod_data_source_block           rj_101c
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7712857
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C64 H40 B4 F16 N8 Pd2'
_shelx_estimated_absorpt_t_max   0.745
_shelx_estimated_absorpt_t_min   0.454
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.755(9)
 0.245(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 F13-F15 \\sim F13-F16 \\sim F13-F14 \\sim F15-F16 \\sim F16-F14
 with sigma of 0.02
 F7-F5 \\sim F7-F6 \\sim F5-F6 \\sim F5-F8 \\sim F6-F8
 with sigma of 0.02
 B4-F13 \\sim B4-F15 \\sim B4-F16 \\sim B4-F14
 with sigma of 0.02
 F28-F25 \\sim F28-F27 \\sim F28-F26 \\sim F25-F27 \\sim F25-F26 \\sim F27-F26
 with sigma of 0.02
 F12-F11 \\sim F12-F9 \\sim F12-F10 \\sim F11-F9 \\sim F11-F10 \\sim F9-F10
 with sigma of 0.02
 F23-F21 \\sim F23-F22 \\sim F21-F22 \\sim F24-F22
 with sigma of 0.02
 F17-F20 \\sim F19-F20 \\sim F19-F18 \\sim F20-F18
 with sigma of 0.02
 B3-F12 \\sim B3-F11 \\sim B3-F9 \\sim B3-F10
 with sigma of 0.02
 B6-F23 \\sim B6-F21 \\sim B6-F24 \\sim B6-F22
 with sigma of 0.02
 B2-F7 \\sim B2-F5 \\sim B2-F6 \\sim B2-F8
 with sigma of 0.02
 B8-F29 \\sim B8-F31 \\sim B8-F32 \\sim B8-F30
 with sigma of 0.02
 B7-F28 \\sim B7-F25 \\sim B7-F27 \\sim B7-F26
 with sigma of 0.02
 F2-F3 \\sim F2-F1 \\sim F2-F4 \\sim F3-F1 \\sim F3-F4 \\sim F1-F4
 with sigma of 0.04
 B5-F17 \\sim B5-F19 \\sim B5-F20 \\sim B5-F18
 with sigma of 0.02
 B1-F2 \\sim B1-F3 \\sim B1-F1 \\sim B1-F4
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Y: Pd1(0.297549)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C13(H13),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C29(H29), C30(H30), C31(H31), C33(H33), C37(H37), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C49(H49), C50(H50), C51(H51),
  C52(H52), C53(H53), C54(H54), C55(H55), C57(H57), C61(H61), C62(H62),
 C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C69(H69), C73(H73), C74(H74),
  C75(H75), C77(H77), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85),
 C86(H86), C87(H87), C89(H89), C93(H93), C94(H94), C95(H95), C97(H97),
 C101(H101), C102(H102), C103(H103), C104(H104), C105(H105), C106(H106),
 C107(H107), C109(H109), C113(H113), C114(H114), C115(H115), C116(H116),
 C117(H117), C118(H118), C119(H119), C121(H121), C125(H125), C126(H126),
 C127(H127), C128(H128)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19644
_shelx_hkl_checksum              89497
_shelx_fab_checksum              11564
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.755
_oxdiff_exptl_absorpt_empirical_full_min 0.385