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_1544631
_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
'C208 H240 B16 Fe8 N56 O48 Pd2, 9(C2 H3 N), 4(B F4)'
_chemical_formula_sum            'C226 H267 B20 F16 Fe8 N65 O48 Pd2'
_chemical_formula_weight         5841.83
_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   mixed
_audit_creation_date             2016-08-17
_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                63.610(5)
_cell_angle_beta                 76.958(5)
_cell_angle_gamma                85.618(5)
_cell_formula_units_Z            1
_cell_length_a                   20.2193(12)
_cell_length_b                   20.6255(11)
_cell_length_c                   21.5175(12)
_cell_measurement_reflns_used    12370
_cell_measurement_temperature    140.0(1)
_cell_measurement_theta_max      61.9100
_cell_measurement_theta_min      4.2600
_cell_volume                     7828.1(9)
_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  'SHELXL-2014 (Sheldrick, 2015a)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015b)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.972
_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  0.0506
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 0.899
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46789
_diffrn_reflns_point_group_measured_fraction_full 0.899
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        65.000
_diffrn_reflns_theta_max         62.048
_diffrn_reflns_theta_min         3.235
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.465
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.294
_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    1.239
_exptl_crystal_description       needle
_exptl_crystal_F_000             3006
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN/DMSO/diethyl ether '
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.911
_refine_diff_density_min         -2.209
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1683
_refine_ls_number_reflns         23977
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.0958
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+80.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2057
_refine_ls_wR_factor_ref         0.2220
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17759
_reflns_number_total             23977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04732g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1544629--1544635.cif.'
_cod_original_cell_volume        7828.1(8)
_cod_database_code               1544631
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Others
 Fixed Sof: H44C(0.5) H44D(0.5) H44A(0.5) H44B(0.5) C45(0.5) H45A(0.5)
 H45B(0.5) C46(0.5) H46A(0.5) H46B(0.5) H47C(0.5) H47D(0.5) H47A(0.5) H47B(0.5)
 C45A(0.5) H45C(0.5) H45D(0.5) C46A(0.5) H46C(0.5) H46D(0.5) C17S(0.5) N9S(0.5)
 C18S(0.5) H18C(0.5) H18D(0.5) H18E(0.5) F1(0.5) F2(0.5) B9A(0.5) B9B(0.5)
 B10(0.5) F6(0.5) F7(0.5) F8(0.5) F9(0.5) N2S(0.5) C3S(0.5) C4S(0.5) H4SA(0.5)
 H4SB(0.5) H4SC(0.5) C7S(0.5) N4S(0.5) C5S(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5)
 H6SC(0.5) N3S(0.5) C8S(0.5) H8SA(0.5) H8SB(0.5) H8SC(0.5) N7S(0.5) C13S(0.5)
 C14S(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C12S(0.25) H12C(0.25) H12D(0.25)
 H12E(0.25) C11S(0.25) N6S(0.25) B11(0.5) F10(0.5) F11(0.5) F12(0.5) F13(0.5)
 C9S(0.5) C10S(0.5) H10C(0.5) H10D(0.5) H10E(0.5) C15S(0.25) N5S(0.5) N8S(0.25)
 C16S(0.25) H16C(0.25) H16D(0.25) H16E(0.25)
 Fixed Uiso: H3A(0.074) H3B(0.074) H4A(0.093) H4B(0.093) H5A(0.1) H5B(0.1)
 H6A(0.072) H6B(0.072) H9A(0.06) H9B(0.06) H10A(0.086) H10B(0.086) H11A(0.095)
 H11B(0.095) H12A(0.057) H12B(0.057) H15A(0.069) H15B(0.069) H16A(0.089)
 H16B(0.089) H17A(0.099) H17B(0.099) H18A(0.072) H18B(0.072) H19(0.051)
 H21(0.061) H22(0.064) H23(0.054) H25(0.061) H27(0.066) H28(0.071) H29(0.065)
 H32A(0.073) H32B(0.073) H33A(0.085) H33B(0.085) H34A(0.093) H34B(0.093)
 H35A(0.072) H35B(0.072) H38A(0.084) H38B(0.084) H39A(0.084) H39B(0.084)
 H40A(0.084) H40B(0.084) H41A(0.084) H41B(0.084) H44C(0.074) H44D(0.074)
 H44A(0.074) H44B(0.074) H45A(0.076) H45B(0.076) H46A(0.076) H46B(0.076)
 H47C(0.073) H47D(0.073) H47A(0.073) H47B(0.073) H48(0.055) H50(0.063)
 H51(0.072) H52(0.064) H55A(0.062) H55B(0.062) H56A(0.084) H56B(0.084)
 H57A(0.094) H57B(0.094) H58A(0.061) H58B(0.061) H61A(0.099) H61B(0.099)
 H62A(0.099) H62B(0.099) H63A(0.099) H63B(0.099) H64A(0.099) H64B(0.099)
 H67A(0.099) H67B(0.099) H68A(0.099) H68B(0.099) H69A(0.099) H69B(0.099)
 H70A(0.099) H70B(0.099) H71(0.054) H73(0.088) H74(0.103) H75(0.078) H77(0.051)
 H79(0.056) H80(0.062) H81(0.055) H84A(0.06) H84B(0.06) H85A(0.124) H85B(0.124)
 H86A(0.095) H86B(0.095) H87A(0.056) H87B(0.056) H90A(0.064) H90B(0.064)
 H91A(0.079) H91B(0.079) H92A(0.084) H92B(0.084) H93A(0.059) H93B(0.059)
 H96A(0.07) H96B(0.07) H97A(0.096) H97B(0.096) H98A(0.122) H98B(0.122)
 H99A(0.069) H99B(0.069) H100(0.053) H102(0.055) H103(0.06) H104(0.054)
 H45C(0.076) H45D(0.076) H46C(0.076) H46D(0.076) H2SA(0.182) H2SB(0.182)
 H2SC(0.182) H18C(0.124) H18D(0.124) H18E(0.124) F1(0.12) H4SA(0.102)
 H4SB(0.102) H4SC(0.102) H6SA(0.163) H6SB(0.163) H6SC(0.163) H8SA(0.123)
 H8SB(0.123) H8SC(0.123) H14A(0.14) H14B(0.14) H14C(0.14) H12C(0.097)
 H12D(0.097) H12E(0.097) B11(0.12) F10(0.12) F11(0.12) F12(0.12) F13(0.12)
 H10C(0.128) H10D(0.128) H10E(0.128) H16C(0.084) H16D(0.084) H16E(0.084)
 Fixed X: H3A(-0.0834) H3B(-0.1427) H4A(-0.1478) H4B(-0.067) H5A(-0.1154) H5B(-
 0.1476) H6A(-0.0501) H6B(-0.006) H9A(-0.0619) H9B(-0.1262) H10A(-0.1204) H10B(-
 0.1324) H11A(-0.0539) H11B(-0.0071) H12A(0.0449) H12B(-0.0254) H15A(0.2637)
 H15B(0.2673) H16A(0.2885) H16B(0.338) H17A(0.2889) H17B(0.2631) H18A(0.1673)
 H18B(0.1855) H19(0.1942) H21(0.1059) H22(0.1755) H23(0.2479) H25(-0.0898) H27(-
 0.1634) H28(-0.1154) H29(-0.0586) H32A(-0.4622) H32B(-0.477) H33A(-0.5244)
 H33B(-0.4599) H34A(-0.464) H34B(-0.4594) H35A(-0.3496) H35B(-0.3537) H38A(-
 0.2975) H38B(-0.2306) H39A(-0.1638) H39B(-0.2316) H40A(-0.2623) H40B(-0.1871)
 H41A(-0.1399) H41B(-0.2061) H44C(-0.0299) H44D(-0.0624) H45A(-0.1047) H45B(-
 0.0245) H46A(-0.0722) H46B(-0.0518) H47C(-0.1585) H47D(-0.1861) H48(-0.2779)
 H50(-0.4615) H51(-0.5071) H52(-0.4404) H55A(0.178) H55B(0.1576) H56A(0.0706)
 H56B(0.1222) H57A(0.0697) H57B(0.1001) H58A(0.1713) H58B(0.1733) H61A(0.3997)
 H61B(0.46) H62A(0.5347) H62B(0.5007) H63A(0.4951) H63B(0.4196) H64A(0.4949)
 H64B(0.4182) H67A(0.5436) H67B(0.4765) H68A(0.4832) H68B(0.5596) H69A(0.5624)
 H69B(0.584) H70A(0.5084) H70B(0.4573) H71(0.3162) H73(0.4452) H74(0.4512)
 H75(0.3875) H77(0.2623) H79(0.3488) H80(0.4529) H81(0.4601) H84A(-0.1051)
 H84B(-0.0962) H85A(-0.0572) H85B(-0.1027) H86A(-0.0119) H86B(-0.0011)
 H87A(0.0813) H87B(0.0969) H90A(-0.0012) H90B(0.0525) H91A(0.0749) H91B(0.0659)
 H92A(0.1797) H92B(0.1774) H93A(0.2271) H93B(0.1749) H96A(0.0703) H96B(0.0301)
 H97A(0.1195) H97B(0.1206) H98A(0.208) H98B(0.2263) H99A(0.2575) H99B(0.2285)
 H100(-0.1495) H102(-0.1186) H103(-0.2284) H104(-0.2954) H45C(-0.0291) H45D(-
 0.0073) H46C(-0.1165) H46D(-0.0795) H2SA(0.3335) H2SB(0.2896) H2SC(0.2524)
 H18C(0.3498) H18D(0.3474) H18E(0.3546) H4SA(0.3754) H4SB(0.3558) H4SC(0.3044)
 H6SA(0.4385) H6SB(0.4769) H6SC(0.4633) H8SA(0.2155) H8SB(0.2265) H8SC(0.1769)
 H14A(-0.25) H14B(-0.174) H14C(-0.2259) H12C(-0.2634) H12D(-0.2515) H12E(-
 0.2827) H10C(0.3901) H10D(0.363) H10E(0.3461) H16C(-0.4348) H16D(-0.373) H16E(-
 0.3631)
 Fixed Y: H3A(0.5752) H3B(0.5443) H4A(0.6666) H4B(0.6769) H5A(0.6948)
 H5B(0.6143) H6A(0.6079) H6B(0.6529) H9A(0.1907) H9B(0.2421) H10A(0.1548)
 H10B(0.2363) H11A(0.1835) H11B(0.1655) H12A(0.265) H12B(0.3032) H15A(0.4847)
 H15B(0.4008) H16A(0.4647) H16B(0.4122) H17A(0.3492) H17B(0.3125) H18A(0.3221)
 H18B(0.4052) H19(0.4082) H21(0.6) H22(0.6364) H23(0.5563) H25(0.2369)
 H27(0.2861) H28(0.4036) H29(0.4375) H32A(0.0102) H32B(0.057) H33A(0.1194)
 H33B(0.1093) H34A(0.2289) H34B(0.1992) H35A(0.2354) H35B(0.1997) H38A(-0.069)
 H38B(-0.1122) H39A(-0.0422) H39B(-0.0498) H40A(0.0621) H40B(0.0651)
 H41A(0.0922) H41B(0.1406) H44C(0.0038) H44D(0.0676) H45A(-0.0154) H45B(-
 0.0266) H46A(-0.1406) H46B(-0.1163) H47C(-0.1659) H47D(-0.128) H48(-0.2458)
 H50(-0.1606) H51(-0.2787) H52(-0.3762) H55A(0.1054) H55B(0.0663) H56A(0.1427)
 H56B(0.2083) H57A(0.2256) H57B(0.1519) H58A(0.2394) H58B(0.2841) H61A(-0.0526)
 H61B(-0.0463) H62A(0.0087) H62B(-0.0597) H63A(0.0407) H63B(0.0171)
 H64A(0.1423) H64B(0.1371) H67A(0.1584) H67B(0.1585) H68A(0.2811) H68B(0.2558)
 H69A(0.358) H69B(0.2906) H70A(0.3506) H70B(0.3606) H71(0.3193) H73(0.4254)
 H74(0.5192) H75(0.5126) H77(-0.0441) H79(-0.2306) H80(-0.1876) H81(-0.0751)
 H84A(-0.1406) H84B(-0.0877) H85A(-0.0612) H85B(-0.012) H86A(0.0278)
 H86B(0.0415) H87A(-0.0406) H87B(-0.0009) H90A(-0.4416) H90B(-0.4799) H91A(-
 0.5252) H91B(-0.4488) H92A(-0.4812) H92B(-0.4831) H93A(-0.3727) H93B(-0.3575)
 H96A(-0.2804) H96B(-0.2068) H97A(-0.1374) H97B(-0.203) H98A(-0.2523) H98B(-
 0.1694) H99A(-0.2183) H99B(-0.1384) H100(-0.3551) H102(-0.305) H103(-0.3515)
 H104(-0.3964) H45C(-0.088) H45D(-0.0526) H46C(-0.0799) H46D(-0.1518) H2SA(-
 0.1593) H2SB(-0.2263) H2SC(-0.1566) H18C(0.1463) H18D(0.1809) H18E(0.2323)
 H4SA(-0.0872) H4SB(-0.0215) H4SC(-0.0894) H6SA(-0.3157) H6SB(-0.345) H6SC(-
 0.2603) H8SA(0.0556) H8SB(-0.0104) H8SC(0.0533) H14A(0.4148) H14B(0.3939)
 H14C(0.3336) H12C(0.365) H12D(0.3919) H12E(0.4454) H10C(0.0004) H10D(0.0686)
 H10E(0.0595) H16C(0.1297) H16D(0.1229) H16E(0.1017)
 Fixed Z: H3A(0.427) H3B(0.4083) H4A(0.3462) H4B(0.322) H5A(0.2259)
 H5B(0.2685) H6A(0.1909) H6B(0.2126) H9A(0.4645) H9B(0.4537) H10A(0.4052)
 H10B(0.3518) H11A(0.2937) H11B(0.3498) H12A(0.2548) H12B(0.2393) H15A(0.2843)
 H15B(0.3016) H16A(0.3881) H16B(0.3637) H17A(0.4846) H17B(0.4423) H18A(0.5212)
 H18B(0.4978) H19(0.1342) H21(0.0747) H22(-0.0381) H23(-0.0638) H25(0.6142)
 H27(0.7782) H28(0.7098) H29(0.5922) H32A(0.9483) H32B(0.8707) H33A(0.9333)
 H33B(0.9681) H34A(0.88) H34B(0.822) H35A(0.807) H35B(0.8908) H38A(0.6862)
 H38B(0.7073) H39A(0.6031) H39B(0.5804) H40A(0.5651) H40B(0.5201) H41A(0.5915)
 H41B(0.5824) H44C(0.8701) H44D(0.8894) H45A(1.006) H45B(0.9859) H46A(1.0343)
 H46B(0.9506) H47C(0.9826) H47D(1.0342) H48(0.9344) H50(0.9561) H51(1.025)
 H52(1.0378) H55A(0.577) H55B(0.5338) H56A(0.5415) H56B(0.5189) H57A(0.4271)
 H57B(0.4269) H58A(0.3347) H58B(0.3791) H61A(0.3763) H61B(0.4107) H62A(0.2983)
 H62B(0.2994) H63A(0.1919) H63B(0.238) H64A(0.2048) H64B(0.199) H67A(0.5117)
 H67B(0.568) H68A(0.5279) H68B(0.5314) H69A(0.4242) H69B(0.4068) H70A(0.3377)
 H70B(0.4014) H71(0.158) H73(0.1988) H74(0.0848) H75(0.0113) H77(0.657)
 H79(0.7709) H80(0.6897) H81(0.5937) H84A(0.7911) H84B(0.8253) H85A(0.6819)
 H85B(0.7139) H86A(0.7305) H86B(0.6498) H87A(0.6604) H87B(0.705) H90A(0.8976)
 H90B(0.9468) H91A(0.8668) H91B(0.8025) H92A(0.7948) H92B(0.8704) H93A(0.7907)
 H93B(0.74) H96A(1.107) H96B(1.0754) H97A(1.0546) H97B(1.1304) H98A(1.0847)
 H98B(1.0601) H99A(0.9724) H99B(0.9474) H100(0.9526) H102(1.1042) H103(1.1692)
 H104(1.124) H45C(0.9243) H45D(0.9695) H46C(1.0444) H46D(1.0448) H2SA(0.5742)
 H2SB(0.6392) H2SC(0.5913) H18C(0.644) H18D(0.5616) H18E(0.5978) H4SA(0.7909)
 H4SB(0.8115) H4SC(0.843) H6SA(0.8417) H6SB(0.9062) H6SC(0.8659) H8SA(0.809)
 H8SB(0.7881) H8SC(0.7528) H14A(0.4976) H14B(0.5078) H14C(0.5173) H12C(0.915)
 H12D(0.8311) H12E(0.8652) H10C(0.9576) H10D(0.8968) H10E(0.9766) H16C(0.7116)
 H16D(0.6536) H16E(0.732)
;
_shelx_res_checksum              83667
_shelx_hkl_checksum              42515
_shelx_fab_checksum              63270
_olex2_submission_special_instructions 'No special instructions were received'