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_7712855
_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         'C96 H64 N16 Pd4, 8[BF4]'
_chemical_formula_sum            'C96 H64 N16 Pd4'
_chemical_formula_weight         1867.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-09-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2023-01-24 deposited with the CCDC.	2023-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.824(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.1944(18)
_cell_length_b                   18.4331(18)
_cell_length_c                   17.3971(12)
_cell_measurement_reflns_used    7365
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      23.2820
_cell_measurement_theta_min      3.6230
_cell_volume                     8698.8(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.78a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.78a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.78a (Rigaku OD, 2020)'
_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)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -51.00  68.00   1.00  100.00    --   -9.76  19.00 150.00  119
  2  \w    -36.00  23.00   1.00  100.00    --   -9.76 -77.00 120.00   59
  3  \w     61.00  98.00   1.00  100.00    --   10.62 178.00   0.00   37
;
_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      -0.0112535000
_diffrn_orient_matrix_UB_12      0.0337647000
_diffrn_orient_matrix_UB_13      0.0037597000
_diffrn_orient_matrix_UB_21      -0.0088996000
_diffrn_orient_matrix_UB_22      -0.0145757000
_diffrn_orient_matrix_UB_23      0.0311458000
_diffrn_orient_matrix_UB_31      0.0218500000
_diffrn_orient_matrix_UB_32      0.0114621000
_diffrn_orient_matrix_UB_33      0.0284476000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23318
_diffrn_reflns_point_group_measured_fraction_full 0.845
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.038
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.41.78a (Rigaku Oxford Diffraction, 2020)
 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    0.713
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.156
_refine_diff_density_rms         0.025
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.422(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.823
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         14777
_refine_ls_number_restraints     880
_refine_ls_restrained_S_all      0.808
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0340P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.617
_reflns_Friedel_fraction_full    0.684
_reflns_Friedel_fraction_max     0.656
_reflns_number_gt                9177
_reflns_number_total             14777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00248a2.cif
_cod_data_source_block           rj-08-bf4
_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               7712855
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C96 H64 N16 Pd4 B6 F24'
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.812
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.578(15)
 0.422(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C48-C48_$1
 1.2 with sigma of 0.005
 C42-C42_$1
 1.2 with sigma of 0.005
 C31-C30
 1.2 with sigma of 0.01
 C7-C6 = C18-C19
 1.2 with sigma of 0.005
 C33-C31 \\sim C31-C36
 with sigma of 0.005
 C29-C30 \\sim C30-C27
 with sigma of 0.01
 C30-C28 \\sim C32-C31
 with sigma of 0.005
 C18-C16 \\sim C20-C19 \\sim C8-C7 \\sim C6-C4
 with sigma of 0.01
4. Restrained planarity
 C28, C30, C31, C32
 with sigma of 0.005
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Uanis(N7) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(C48) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
6. 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
7.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C2(H2), C1(H1), C13(H13), C14(H14), C15(H15), C17(H17),
 C25(H25), C26(H26), C27(H27), C29(H29), C37(H37), C38(H38), C39(H39), C41(H41),
  C11(H11), C10(H10), C9(H9), C12(H12), C24(H24), C21(H21), C22(H22), C23(H23),
 C43(H43), C45(H45), C46(H46), C47(H47), C33(H33), C36(H36), C35(H35), C34(H34)
7.b Fitted hexagon refined as free rotating group:
 N1(C5,C4,C3,C2,C1), N2(C13,C14,C15,C16,C17), N3(C25,C26,C27,C28,C29), N4(C37,
 C38,C39,C40,C41), N5(C11,C10,C9,C8,C12), N6(C24,C20,C21,C22,C23), N7(C43,C44,
 C45,C46,C47), N8(C33,C32,C36,C35,C34)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30505
_shelx_hkl_checksum              98102
_shelx_fab_checksum              43087
_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 1.816
_oxdiff_exptl_absorpt_empirical_full_min 0.624