PdII2L4-type coordination cages up to three nanometers in size
Jansze, Suzanne M.; Wise, Matthew D.; Vologzhanina, Anna V.; Scopelliti, Rosario; Severin, Kay; Chem. Sci. 8 (2017) 1901–; doi:10.1039/C6SC04732G

data_1544635
_publ_section_title
;
 PdII2L4-type coordination cages up to three nanometers in size
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              1901
_journal_paper_doi               10.1039/C6SC04732G
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety
'C252 H288 B16 Fe8 N56 O56 Pd2, 6(C2 H3 N), 4(B F4)'
_chemical_formula_sum            'C264 H306 B20 F16 Fe8 N62 O56 Pd2'
_chemical_formula_weight         6423.49
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_Hall           '-P 4 2n'
_space_group_name_H-M_alt        'P 4/m n c'
_symmetry_space_group_name_Hall  '-P 4 2n'
_symmetry_space_group_name_H-M   'P 4/m n c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-10-21 deposited with the CCDC.
2016-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.54710(8)
_cell_length_b                   17.54710(8)
_cell_length_c                   62.6742(5)
_cell_measurement_reflns_used    70241
_cell_measurement_temperature    140.0(1)
_cell_measurement_theta_max      75.3940
_cell_measurement_theta_min      3.7480
_cell_volume                     19297.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2015a)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015b)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -77
_diffrn_reflns_number            140802
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.652
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.678
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       prism
_exptl_crystal_F_000             6632
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN/DMSO/diethyl ether '
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.396
_refine_diff_density_min         -2.214
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         10092
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0700P)^2^+59.4447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1667
_reflns_number_gt                9604
_reflns_number_total             10092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04732g2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 1544629--1544635.cif.'
_cod_database_code               1544635
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Others
 Fixed Sof: C1S(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5) H2SC(0.5) F2(0.5) N1S(0.5)
 F1(0.5) B3(0.25) N2S(0.25) C4S(0.25) H4SA(0.25) H4SB(0.25) H4SC(0.25)
 C3S(0.25) B4(0.25) F5(0.25) F4(0.25) F6(0.25)
 Fixed U12: Pd1(0)
 Fixed U13: Pd1(0) C32(0)
 Fixed U23: Pd1(0) C32(0)
 Fixed Uiso: H3A(0.047) H3B(0.047) H4A(0.079) H4B(0.079) H5A(0.077) H5B(0.077)
 H6A(0.045) H6B(0.045) H9A(0.045) H9B(0.045) H10A(0.077) H10B(0.077)
 H11A(0.077) H11B(0.077) H12A(0.049) H12B(0.049) H15A(0.052) H15B(0.052)
 H16A(0.06) H16B(0.06) H17A(0.057) H17B(0.057) H18A(0.05) H18B(0.05) H21(0.044)
 H22(0.046) H23(0.041) H25(0.05) H26(0.051) H28(0.049) H29(0.046) H30A(0.061)
 H30B(0.061) H31A(0.064) H31B(0.064) H32A(0.058) H32B(0.058) H2SA(0.104)
 H2SB(0.104) H2SC(0.104) F2(0.08) F1(0.08) B3(0.08) H4SA(0.061) H4SB(0.061)
 H4SC(0.061) B4(0.084) F5(0.06) F4(0.06) F6(0.06)
 Fixed X: Pd1(0) H3A(0.2734) H3B(0.1944) H4A(0.124) H4B(0.1901) H5A(0.257)
 H5B(0.1759) H6A(0.1248) H6B(0.2069) H9A(0.4612) H9B(0.4803) H10A(0.5512)
 H10B(0.5741) H11A(0.4978) H11B(0.5581) H12A(0.4688) H12B(0.4264) H15A(0.0635)
 H15B(0.1042) H16A(-0.0242) H16B(-0.0227) H17A(-0.0168) H17B(0.0629)
 H18A(0.0953) H18B(0.0344) H21(0.3155) H22(0.2791) H23(0.151) H25(0.2025)
 H26(0.2105) H28(0.3775) H29(0.3683) H30A(0.3987) H30B(0.3358) H31A(0.3625)
 H31B(0.2767) H32A(0.4019) H32B(0.3162) H2SA(0.5017) H2SB(0.4943) H2SC(0.4266)
 H4SA(0.1775) H4SB(0.1799) H4SC(0.2343) F3(0.5)
 Fixed Y: Pd1(0) H3A(0.0799) H3B(0.1238) H4A(0.022) H4B(-0.016) H5A(-0.0447)
 H5B(-0.0861) H6A(-0.0058) H6B(-0.0288) H9A(0.3759) H9B(0.3183) H10A(0.242)
 H10B(0.3253) H11A(0.3128) H11B(0.2447) H12A(0.1574) H12B(0.212) H15A(0.3898)
 H15B(0.4461) H16A(0.439) H16B(0.3478) H17A(0.396) H17B(0.4357) H18A(0.3235)
 H18B(0.2756) H21(0.0689) H22(-0.002) H23(-0.0266) H25(0.3138) H26(0.3924)
 H28(0.5149) H29(0.4349) H30A(0.5506) H30B(0.6021) H31A(0.6574) H31B(0.627)
 H32A(0.5491) H32B(0.5177) H2SA(0.1713) H2SB(0.1979) H2SC(0.2147) H4SA(0.2403)
 H4SB(0.3184) H4SC(0.2492) F3(0.5)
 Fixed Z: H3A(0.0955) H3B(0.0921) H4A(0.1025) H4B(0.0885) H5A(0.1198)
 H5B(0.1189) H6A(0.1441) H6B(0.1533) H9A(0.1597) H9B(0.1406) H10A(0.1614)
 H10B(0.1694) H11A(0.199) H11B(0.198) H12A(0.1908) H12B(0.2074) H15A(0.1359)
 H15B(0.1525) H16A(0.1625) H16B(0.1618) H17A(0.1975) H17B(0.1919) H18A(0.2085)
 H18B(0.195) H21(0.2291) H22(0.2591) H23(0.2653) H25(0.0775) H26(0.0478)
 H28(0.0766) H29(0.1063) H30A(0.0412) H30B(0.053) H31A(0.0199) H31B(0.0197)
 C32(0) H32A(0) H32B(0) H2SA(0.0952) H2SB(0.1196) H2SC(0.1031) B3(0.25)
 H4SA(0.2415) H4SB(0.2547) H4SC(0.2613)
;
_shelx_res_checksum              97724
_shelx_hkl_checksum              74375
_shelx_fab_checksum              81541
_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 1.417
_oxdiff_exptl_absorpt_empirical_full_min 0.675