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_1544633
_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
'C236 H256 B16 Fe8 N56 O48 Pd2, 4(B F4), 1.5(C6 H14 O), 8(C2 H3 N), 0.5(C2 H6 O S)'
_chemical_formula_sum            'C262 H304 B20 F16 Fe8 N64 O50 Pd2 S0.5'
_chemical_formula_weight         6345.50
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_date             2016-08-19
_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                105.440(4)
_cell_angle_beta                 91.132(3)
_cell_angle_gamma                90.267(3)
_cell_formula_units_Z            1
_cell_length_a                   21.3764(8)
_cell_length_b                   21.4422(9)
_cell_length_c                   23.5362(10)
_cell_measurement_reflns_used    14847
_cell_measurement_temperature    140.0(1)
_cell_measurement_theta_max      73.6340
_cell_measurement_theta_min      3.8550
_cell_volume                     10396.1(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_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 0.958
_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  0.0536
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            78249
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         76.743
_diffrn_reflns_theta_min         3.821
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.422
_exptl_absorpt_correction_T_max  0.200
_exptl_absorpt_correction_T_min  0.042
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.014
_exptl_crystal_description       prism
_exptl_crystal_F_000             3276
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN/DMSo / isopropyl ether '
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.106
_refine_diff_density_min         -2.069
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1998
_refine_ls_number_reflns         41971
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1317
_refine_ls_R_factor_gt           0.0979
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+60.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2092
_refine_ls_wR_factor_ref         0.2274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28354
_reflns_number_total             41971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04732g2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1544629--1544635.cif.'
_cod_original_cell_volume        10396.1(7)
_cod_original_formula_sum        'C262 H304 B20 F16 Fe8 N64 O50 Pd2 S0.50'
_cod_database_code               1544633
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Others
 Fixed Sof: O204(0.5) N1S(0.5) N3S(0.5) C1S(0.5) C212(0.5) H21A(0.5) H21B(0.5)
 H21C(0.5) C5S(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) H2SC(0.5) C218(0.5) H21D(0.5) H21E(0.5) H21F(0.5) C219(0.5)
 H219(0.5) C221(0.5) H221(0.5) C224(0.5) H22A(0.5) H22B(0.5) H22C(0.5)
 C225(0.5) H22D(0.5) H22E(0.5) H22F(0.5) F7(0.5) F8(0.5) F5(0.5) F6(0.5)
 C10S(0.5) H10O(0.5) H10P(0.5) H10Q(0.5) C9S(0.5) N5S(0.5) C12S(0.5) H12C(0.5)
 H12D(0.5) H12E(0.5) C11S(0.5) N6S(0.5) C25S(0.25) H25A(0.25) H25B(0.25)
 H25C(0.25) C24S(0.25) H24S(0.25) C23S(0.25) H23A(0.25) H23B(0.25) H23C(0.25)
 O0AA(0.25) C22S(0.25) H22G(0.25) H22H(0.25) H22I(0.25) C21S(0.25) H21S(0.25)
 C26S(0.25) H26A(0.25) H26B(0.25) H26C(0.25) C19S(0.25) H19A(0.25) H19B(0.25)
 H19C(0.25) S1S(0.25) C20S(0.25) H20A(0.25) H20B(0.25) H20C(0.25) O3S(0.25)
 F8A(0.5) F5A(0.5) F6A(0.5) F7A(0.5)
 Fixed Uiso: H3A(0.072) H3B(0.072) H4A(0.147) H4B(0.147) H5(0.117) H6A(0.069)
 H6B(0.069) H9A(0.073) H9B(0.073) H10A(0.078) H10B(0.078) H11A(0.076)
 H11B(0.076) H12A(0.074) H12B(0.074) H15A(0.073) H15B(0.073) H16A(0.084)
 H16B(0.084) H17A(0.083) H17B(0.083) H18A(0.071) H18B(0.071) H19(0.061)
 H21(0.085) H22(0.089) H23(0.073) H25(0.076) H26(0.076) H28(0.067) H29(0.069)
 H30A(0.075) H30B(0.075) H33(0.107) H39A(0.082) H39B(0.082) H40A(0.136)
 H40B(0.136) H41A(0.11) H41B(0.11) H42A(0.095) H42B(0.095) H45A(0.075)
 H45B(0.075) H46A(0.093) H46B(0.093) H47A(0.099) H47B(0.099) H48A(0.084)
 H48B(0.084) H51A(0.099) H51B(0.099) H52A(0.148) H52B(0.148) H53A(0.173)
 H53B(0.173) H54A(0.093) H54B(0.093) H55(0.062) H57(0.079) H58(0.083)
 H59(0.069) H62A(0.067) H62B(0.067) H63A(0.082) H63B(0.082) H64A(0.075)
 H64B(0.075) H65A(0.067) H65B(0.067) H68A(0.069) H68B(0.069) H69A(0.089)
 H69B(0.089) H70A(0.08) H70B(0.08) H71A(0.067) H71B(0.067) H74A(0.068)
 H74B(0.068) H75A(0.126) H75B(0.126) H76A(0.103) H76B(0.103) H77A(0.069)
 H77B(0.069) H78(0.057) H80(0.066) H81(0.066) H82(0.059) H84(0.079) H85(0.083)
 H87(0.103) H88(0.098) H89A(0.078) H89B(0.078) H91(0.078) H92(0.076) H94(0.081)
 H95(0.082) H98A(0.07) H98B(0.07) H99A(0.079) H99B(0.079) H10C(0.085)
 H10D(0.085) H10E(0.087) H10F(0.087) H10G(0.1) H10H(0.1) H10I(0.142)
 H10J(0.142) H10K(0.141) H10L(0.141) H10M(0.091) H10N(0.091) H11C(0.082)
 H11D(0.082) H11E(0.092) H11F(0.092) H11G(0.093) H11H(0.093) H11I(0.085)
 H11J(0.085) H114(0.063) H116(0.074) H117(0.079) H118(0.069) H4SA(0.154)
 H4SB(0.154) H4SC(0.154) H8SA(0.149) H8SB(0.149) H8SC(0.149) H21A(0.082)
 H21B(0.082) H21C(0.082) H6SA(0.098) H6SB(0.098) H6SC(0.098) H2SA(0.098)
 H2SB(0.098) H2SC(0.098) H21D(0.104) H21E(0.104) H21F(0.104) H219(0.071)
 H221(0.101) H22A(0.142) H22B(0.142) H22C(0.142) H22D(0.153) H22E(0.153)
 H22F(0.153) F7(0.08) F8(0.08) B6(0.08) F5(0.08) F6(0.08) H10O(0.129)
 H10P(0.129) H10Q(0.129) H12C(0.132) H12D(0.132) H12E(0.132) H25A(0.059)
 H25B(0.059) H25C(0.059) H24S(0.087) H23A(0.092) H23B(0.092) H23C(0.092)
 H22G(0.094) H22H(0.094) H22I(0.094) H21S(0.099) H26A(0.123) H26B(0.123)
 H26C(0.123) H19A(0.257) H19B(0.257) H19C(0.257) H20A(0.257) H20B(0.257)
 H20C(0.257) F8A(0.08) F5A(0.08) F6A(0.08) F7A(0.08)
 Fixed X: H3A(0.6401) H3B(0.6073) H4A(0.7137) H4B(0.6954) H5(0.7943)
 H6A(0.7768) H6B(0.761) H9A(0.4915) H9B(0.4422) H10A(0.4854) H10B(0.4855)
 H11A(0.5915) H11B(0.582) H12A(0.5907) H12B(0.6497) H15A(0.4109) H15B(0.4573)
 H16A(0.431) H16B(0.432) H17A(0.5196) H17B(0.5431) H18A(0.5983) H18B(0.5343)
 H19(0.7283) H21(0.7694) H22(0.843) H23(0.8596) H25(0.3574) H26(0.2777)
 H28(0.3772) H29(0.4577) H30A(0.225) H30B(0.2683) H33(0.3299) H39A(0.3368)
 H39B(0.3784) H40A(0.4538) H40B(0.4289) H41A(0.3816) H41B(0.4516) H42A(0.3708)
 H42B(0.4217) H45A(0.2686) H45B(0.201) H46A(0.2674) H46B(0.3197) H47A(0.2693)
 H47B(0.2042) H48A(0.2356) H48B(0.3068) H51A(0.0619) H51B(0.028) H52A(0.0237)
 H52B(-0.0298) H53A(-0.0107) H53B(0.0008) H54A(0.0717) H54B(0.0962) H55(0.2032)
 H57(0.1817) H58(0.1601) H59(0.1587) H62A(0.4833) H62B(0.4479) H63A(0.5403)
 H63B(0.5481) H64A(0.6062) H64B(0.6378) H65A(0.6134) H65B(0.6335) H68A(0.2836)
 H68B(0.2678) H69A(0.2783) H69B(0.3397) H70A(0.3627) H70B(0.3354) H71A(0.4416)
 H71B(0.449) H74A(0.3161) H74B(0.3546) H75A(0.414) H75B(0.3491) H76A(0.3829)
 H76B(0.4331) H77A(0.5053) H77B(0.4742) H78(0.6767) H80(0.575) H81(0.666)
 H82(0.7609) H84(0.2172) H85(0.1251) H87(0.2038) H88(0.2971) H89A(0.0602)
 H89B(0.0796) H91(0.0695) H92(0.067) H94(0.1183) H95(0.1221) H98A(0.0431)
 H98B(0.1151) H99A(0.06) H99B(0.0088) H10C(0.1375) H10D(0.0817) H10E(0.1127)
 H10F(0.039) H10G(-0.121) H10H(-0.0882) H10I(-0.1853) H10J(-0.1339) H10K(-
 0.1652) H10L(-0.1699) H10M(-0.0917) H10N(-0.0693) H11C(0.2332) H11D(0.2046)
 H11E(0.3067) H11F(0.3067) H11G(0.3104) H11H(0.2438) H11I(0.2208) H11J(0.2674)
 H114(0.1483) H116(-0.0373) H117(-0.0382) H118(0.0549) H4SA(0.3849)
 H4SB(0.3331) H4SC(0.3327) H8SA(0.1339) H8SB(0.1931) H8SC(0.1262) H21A(0.0244)
 H21B(-0.0432) H21C(0.0179) H6SA(0.2976) H6SB(0.2516) H6SC(0.2258) H2SA(0.5463)
 H2SB(0.5458) H2SC(0.5323) H21D(-0.0097) H21E(-0.0617) H21F(0.0054) H219(-
 0.0188) H221(0.0861) H22A(0.1846) H22B(0.1932) H22C(0.1945) H22D(0.0528)
 H22E(0.0708) H22F(0.1225) H10O(0.2201) H10P(0.2363) H10Q(0.2764) H12C(0.2876)
 H12D(0.2256) H12E(0.2202) H25A(0.2259) H25B(0.2652) H25C(0.1937) H24S(0.2146)
 H23A(0.3053) H23B(0.3449) H23C(0.2703) H22G(0.37) H22H(0.3629) H22I(0.3946)
 H21S(0.2665) H26A(0.2335) H26B(0.3068) H26C(0.2643) H19A(0.5898) H19B(0.5429)
 H19C(0.562) H20A(0.4053) H20B(0.422) H20C(0.459)
 Fixed Y: H3A(0.1258) H3B(0.0569) H4A(0.0742) H4B(0.0063) H5(0.0691)
 H6A(0.063) H6B(-0.0098) H9A(0.2453) H9B(0.2027) H10A(0.2311) H10B(0.2973)
 H11A(0.2799) H11B(0.2878) H12A(0.1751) H12B(0.1976) H15A(-0.0875) H15B(-
 0.1219) H16A(-0.2056) H16B(-0.16) H17A(-0.2319) H17B(-0.1958) H18A(-0.1494)
 H18B(-0.1365) H19(0.0672) H21(-0.0869) H22(-0.1178) H23(-0.0525) H25(0.1443)
 H26(0.1662) H28(0.091) H29(0.0676) H30A(0.1339) H30B(0.1129) H33(0.3058)
 H39A(0.5992) H39B(0.6359) H40A(0.5646) H40B(0.5582) H41A(0.4682) H41B(0.464)
 H42A(0.4136) H42B(0.4573) H45A(0.7174) H45B(0.6985) H46A(0.7006) H46B(0.6605)
 H47A(0.5989) H47B(0.6092) H48A(0.5089) H48B(0.5323) H51A(0.5821) H51B(0.5866)
 H52A(0.4902) H52B(0.5144) H53A(0.448) H53B(0.4096) H54A(0.3991) H54B(0.3885)
 H55(0.791) H57(0.7362) H58(0.8416) H59(0.9209) H62A(0.384) H62B(0.3955)
 H63A(0.4044) H63B(0.4495) H64A(0.3707) H64B(0.3916) H65A(0.2954) H65B(0.274)
 H68A(0.2126) H68B(0.1373) H69A(0.149) H69B(0.1932) H70A(0.0889) H70B(0.059)
 H71A(0.063) H71B(0.1329) H74A(0.0833) H74B(0.131) H75A(0.0532) H75B(0.0157)
 H76A(-0.0338) H76B(-0.0438) H77A(0.0181) H77B(-0.023) H78(0.1037) H80(0.0097)
 H81(-0.0414) H82(-0.0177) H84(0.2107) H85(0.2622) H87(0.4315) H88(0.378)
 H89A(0.3531) H89B(0.4079) H91(0.3726) H92(0.4479) H94(0.589) H95(0.5137)
 H98A(0.6157) H98B(0.5951) H99A(0.5027) H99B(0.5114) H10C(0.4797) H10D(0.4273)
 H10E(0.4696) H10F(0.4701) H10G(0.7598) H10H(0.8207) H10I(0.7728) H10J(0.8042)
 H10K(0.7235) H10L(0.68) H10M(0.6321) H10N(0.6955) H11C(0.8208) H11D(0.8559)
 H11E(0.7701) H11F(0.8426) H11G(0.773) H11H(0.8079) H11I(0.7005) H11J(0.6773)
 H114(0.8335) H116(0.8505) H117(0.9328) H118(0.9619) H4SA(-0.2187) H4SB(-
 0.1662) H4SC(-0.2347) H8SA(0.1896) H8SB(0.1557) H8SC(0.1517) H21A(0.2526)
 H21B(0.2814) H21C(0.3262) H6SA(-0.1519) H6SB(-0.0915) H6SC(-0.1602)
 H2SA(0.2756) H2SB(0.3146) H2SC(0.3515) H21D(0.1802) H21E(0.1928) H21F(0.1659)
 H219(0.2919) H221(0.3618) H22A(0.3083) H22B(0.3744) H22C(0.3065) H22D(0.3888)
 H22E(0.3193) H22F(0.3758) H10O(0.1034) H10P(0.0282) H10Q(0.0811) H12C(0.2922)
 H12D(0.3148) H12E(0.2769) H25A(0.4144) H25B(0.4806) H25C(0.4811) H24S(0.4289)
 H23A(0.2453) H23B(0.2672) H23C(0.2614) H22G(0.3194) H22H(0.3958) H22I(0.3528)
 H21S(0.3472) H26A(0.5358) H26B(0.5207) H26C(0.4912) H19A(0.2873) H19B(0.3022)
 H19C(0.2292) H20A(0.3186) H20B(0.3344) H20C(0.3705)
 Fixed Z: H3A(0.5514) H3B(0.5454) H4A(0.5858) H4B(0.5417) H5(0.5316)
 H6A(0.4293) H6B(0.4303) H9A(0.3788) H9B(0.3321) H10A(0.2552) H10B(0.3065)
 H11A(0.3288) H11B(0.2634) H12A(0.2222) H12B(0.2663) H15A(0.334) H15B(0.3703)
 H16A(0.2895) H16B(0.2455) H17A(0.233) H17B(0.2987) H18A(0.2335) H18B(0.2019)
 H19(0.1859) H21(0.2446) H22(0.1712) H23(0.1078) H25(0.438) H26(0.5045)
 H28(0.6158) H29(0.5498) H30A(0.5882) H30B(0.636) H33(0.7679) H39A(1.0213)
 H39B(0.9843) H40A(0.9718) H40B(1.0334) H41A(0.9932) H41B(0.9708) H42A(0.8992)
 H42B(0.8778) H45A(0.7722) H45B(0.7414) H46A(0.6654) H46B(0.6895) H47A(0.6054)
 H47B(0.6388) H48A(0.6452) H48B(0.6603) H51A(0.9619) H51B(0.9018) H52A(0.9577)
 H52B(0.9212) H53A(0.8442) H53B(0.8926) H54A(0.807) H54B(0.8685) H55(0.8917)
 H57(1.0387) H58(1.0879) H59(1.038) H62A(0.2327) H62B(0.1757) H63A(0.1306)
 H63B(0.1965) H64A(0.2232) H64B(0.17) H65A(0.1036) H65B(0.1615) H68A(0.0025)
 H68B(-0.007) H69A(-0.1009) H69B(-0.0827) H70A(-0.1406) H70B(-0.0906) H71A(-
 0.0718) H71B(-0.0835) H74A(0.2262) H74B(0.2794) H75A(0.2952) H75B(0.2766)
 H76A(0.1872) H76B(0.2349) H77A(0.2077) H77B(0.1466) H78(0.1039) H80(-0.0393)
 H81(-0.0796) H82(-0.0271) H84(0.206) H85(0.239) H87(0.235) H88(0.2031)
 H89A(0.2559) H89B(0.2248) H91(0.3611) H92(0.4523) H94(0.3787) H95(0.2864)
 H98A(0.7703) H98B(0.7638) H99A(0.7693) H99B(0.7214) H10C(0.6939) H10D(0.6792)
 H10E(0.5966) H10F(0.6079) H10G(0.6468) H10H(0.6319) H10I(0.58) H10J(0.548)
 H10K(0.4848) H10L(0.5297) H10M(0.4799) H10N(0.4618) H11C(0.6744) H11D(0.6277)
 H11E(0.6119) H11F(0.6057) H11G(0.512) H11H(0.5185) H11I(0.476) H11J(0.5204)
 H114(0.8043) H116(0.7805) H117(0.8695) H118(0.9239) H4SA(-0.0057) H4SB(0.0213)
 H4SC(0.0363) H8SA(0.0678) H8SB(0.0892) H8SC(0.1174) H21A(0.1349) H21B(0.1271)
 H21C(0.1326) H6SA(0.1624) H6SB(0.1727) H6SC(0.1771) H2SA(0.8489) H2SB(0.9171)
 H2SC(0.8673) H21D(-0.011) H21E(0.0387) H21F(0.0512) H219(0.0379) H221(0.091)
 H22A(0.0948) H22B(0.0762) H22C(0.0271) H22D(0.0075) H22E(-0.0336) H22F(-
 0.0163) H10O(0.3313) H10P(0.3192) H10Q(0.367) H12C(0.8783) H12D(0.8504)
 H12E(0.9003) H25A(0.5108) H25B(0.5306) H25C(0.5093) H24S(0.4182) H23A(0.3289)
 H23B(0.3895) H23C(0.3905) H22G(0.3095) H22H(0.3367) H22I(0.3753) H21S(0.3395)
 H26A(0.4368) H26B(0.4365) H26C(0.3787) H19A(0.5245) H19B(0.4761) H19C(0.4723)
 H20A(0.5746) H20B(0.5139) H20C(0.5735)
;
_shelx_res_checksum              36281
_shelx_hkl_checksum              63936
_shelx_fab_checksum              98516
_olex2_submission_special_instructions 'No special instructions were received'