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_1544634
_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         'C244 H264 B16 Fe8 N56 O56 Pd2, 4(B F4)'
_chemical_formula_sum            'C244 H264 B20 F16 Fe8 N56 O56 Pd2'
_chemical_formula_weight         6056.90
_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             2016-08-01
_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                96.416(4)
_cell_angle_beta                 91.400(6)
_cell_angle_gamma                109.195(6)
_cell_formula_units_Z            1
_cell_length_a                   20.6996(19)
_cell_length_b                   21.9894(10)
_cell_length_c                   23.0916(12)
_cell_measurement_reflns_used    6738
_cell_measurement_temperature    140.0(1)
_cell_measurement_theta_max      73.5300
_cell_measurement_theta_min      3.8750
_cell_volume                     9843.2(12)
_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  '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 0.950
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0991
_diffrn_reflns_av_unetI/netI     0.1496
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            74423
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         76.928
_diffrn_reflns_theta_min         3.603
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.576
_exptl_absorpt_correction_T_max  0.639
_exptl_absorpt_correction_T_min  0.393
_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    1.022
_exptl_crystal_description       prism
_exptl_crystal_F_000             3112
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN/DMSO/diethyl ether '
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.177
_refine_diff_density_max         2.280
_refine_diff_density_min         -3.570
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1697
_refine_ls_number_reflns         39511
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.2287
_refine_ls_R_factor_gt           0.1499
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+90.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2913
_refine_ls_wR_factor_ref         0.3359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18393
_reflns_number_total             39518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04732g2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 1544629--1544635.cif.'
_cod_database_code               1544634
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Others
 Fixed Sof: H15A(0.5) H15B(0.5) H15C(0.5) H15D(0.5) C16(0.5) H16A(0.5)
 H16B(0.5) C17(0.5) H17A(0.5) H17B(0.5) H18A(0.5) H18B(0.5) H18C(0.5) H18D(0.5)
 H69A(0.5) H69B(0.5) H69C(0.5) H69D(0.5) C70(0.5) H70A(0.5) H70B(0.5) C71(0.5)
 H71A(0.5) H71B(0.5) H72C(0.5) H72D(0.5) H72A(0.5) H72B(0.5) H11E(0.5)
 H11F(0.5) H11G(0.5) H11H(0.5) C114(0.5) H11I(0.5) H11J(0.5) C115(0.5)
 H11K(0.5) H11L(0.5) H11O(0.5) H11P(0.5) H11M(0.5) H11N(0.5) C16A(0.5)
 H16C(0.5) H16D(0.5) C17A(0.5) H17C(0.5) H17D(0.5) C71A(0.5) H71C(0.5)
 H71D(0.5) C70A(0.5) H70C(0.5) H70D(0.5) C12(0.5) H12A(0.5) H12B(0.5) C1A(0.5)
 H1AA(0.5) H1AB(0.5)
 Fixed Uiso: H0AA(0.093) H0AB(0.093) H3A(0.101) H3B(0.101) H3AA(0.1) H3AB(0.1)
 H3CA(0.107) H4A(0.119) H4B(0.119) H5A(0.114) H5B(0.114) H6A(0.087) H6B(0.087)
 H9A(0.082) H9B(0.082) H10A(0.099) H10B(0.099) H11A(0.094) H11B(0.094)
 H15A(0.127) H15B(0.127) H15C(0.127) H15D(0.127) H16A(0.122) H16B(0.122)
 H17A(0.107) H17B(0.107) H18A(0.143) H18B(0.143) H18C(0.143) H18D(0.143)
 H19(0.068) H21(0.087) H22(0.083) H23(0.085) H25(0.095) H26(0.097) H28(0.121)
 H29(0.096) H35A(0.094) H35B(0.094) H36A(0.143) H36B(0.143) H37A(0.137)
 H37B(0.137) H38A(0.102) H38B(0.102) H41A(0.089) H41B(0.089) H42A(0.096)
 H42B(0.096) H43A(0.086) H43B(0.086) H46A(0.123) H46B(0.123) H47A(0.148)
 H47B(0.148) H48A(0.131) H48B(0.131) H49A(0.107) H49B(0.107) H52(0.163)
 H51(0.163) H55(0.163) H54(0.163) H56(0.075) H58(0.089) H59(0.089) H60(0.077)
 H69A(0.127) H69B(0.127) H69C(0.127) H69D(0.127) H70A(0.094) H70B(0.094)
 H71A(0.128) H71B(0.128) H72C(0.131) H72D(0.131) H72A(0.131) H72B(0.131)
 H75A(0.079) H75B(0.079) H76A(0.098) H76B(0.098) H77A(0.083) H77B(0.083)
 H78A(0.073) H78B(0.073) H79(0.079) H81(0.095) H82(0.105) H83(0.088) H85(0.136)
 H86(0.122) H88(0.132) H89(0.115) H90A(0.137) H90B(0.137) H91A(0.151)
 H91B(0.151) H92A(0.129) H92B(0.129) H94(0.112) H95(0.115) H97(0.092)
 H98(0.082) H10C(0.089) H10D(0.089) H10E(0.091) H10F(0.091) H10G(0.105)
 H10H(0.105) H10I(0.099) H10J(0.099) H10K(0.108) H10L(0.108) H10M(0.144)
 H10N(0.144) H10O(0.123) H10P(0.123) H11C(0.112) H11D(0.112) H11E(0.095)
 H11F(0.095) H11G(0.095) H11H(0.095) H11I(0.08) H11J(0.08) H11K(0.086)
 H11L(0.086) H11O(0.099) H11P(0.099) H11M(0.099) H11N(0.099) H117(0.095)
 H119(0.093) H120(0.089) H16C(0.122) H16D(0.122) H17C(0.107) H17D(0.107)
 H71C(0.128) H71D(0.128) H70C(0.094) H70D(0.094) H12A(0.086) H12B(0.086)
 H1AA(0.08) H1AB(0.08) H32A(0.143) H32B(0.143) H31A(0.123) H31B(0.123)
 H30A(0.136) H30B(0.136) F1(0.08) F3(0.08) B9(0.08) F4(0.08) F2(0.08) F7(0.08)
 F6(0.08) F5(0.08) F8(0.08)
 Fixed X: H0AA(1.105) H0AB(1.1407) H3A(0.5453) H3B(0.4675) H3AA(0.7419)
 H3AB(0.7496) H3CA(1.395) H4A(0.5262) H4B(0.5888) H5A(0.4538) H5B(0.5159)
 H6A(0.4957) H6B(0.5734) H9A(0.6904) H9B(0.628) H10A(0.6568) H10B(0.7283)
 H11A(0.6778) H11B(0.6348) H15A(0.3117) H15B(0.324) H15C(0.2976) H15D(0.3305)
 H16A(0.2112) H16B(0.2307) H17A(0.2128) H17B(0.251) H18A(0.334) H18B(0.3039)
 H18C(0.3364) H18D(0.287) H19(0.6068) H21(0.4034) H22(0.4163) H23(0.5217)
 H25(0.5315) H26(0.5244) H28(0.4521) H29(0.4602) H35A(0.8852) H35B(0.9318)
 H36A(0.8457) H36B(0.8184) H37A(0.7396) H37B(0.7403) H38A(0.7709) H38B(0.7318)
 H41A(1.1421) H41B(1.1187) H42A(1.0418) H42B(1.0243) H43A(0.9374) H43B(0.986)
 H46A(1.0307) H46B(1.0042) H47A(0.8992) H47B(0.9556) H48A(0.9384) H48B(0.8715)
 H49A(0.8149) H49B(0.8541) H52(0.7144) H51(0.8065) H55(0.6747) H54(0.5826)
 H56(1.1861) H58(1.0667) H59(1.1628) H60(1.2642) H69A(0.8946) H69B(0.9478)
 H69C(0.9345) H69D(0.8908) H70A(0.9686) H70B(0.8898) H71A(0.9476) H71B(0.8897)
 H72C(0.8423) H72D(0.8998) H72A(0.8467) H72B(0.8795) H75A(0.5681) H75B(0.5979)
 H76A(0.4861) H76B(0.4796) H77A(0.4701) H77B(0.5473) H78A(0.5521) H78B(0.5038)
 H79(0.6803) H81(0.676) H82(0.6436) H83(0.6468) H85(0.6724) H86(0.6848)
 H88(0.89) H89(0.8742) H90A(0.7052) H90B(0.758) H91A(0.7091) H91B(0.6835)
 H92A(0.7628) H92B(0.8218) H94(0.9526) H95(0.8646) H97(0.8371) H98(0.914)
 H10C(1.1042) H10D(1.1692) H10E(1.1065) H10F(1.0835) H10G(0.9882) H10H(0.9921)
 H10I(1.0119) H10J(0.9534) H10K(1.3265) H10L(1.3147) H10M(1.3543) H10N(1.2846)
 H10O(1.2783) H10P(1.2878) H11C(1.1722) H11D(1.1725) H11E(1.1085) H11F(1.0699)
 H11G(1.0447) H11H(1.1161) H11I(0.9641) H11J(1.0082) H11K(0.9333) H11L(0.928)
 H11O(0.9199) H11P(0.9735) H11M(0.9568) H11N(0.9205) H117(1.2428) H119(1.318)
 H120(1.3989) H16C(0.2324) H16D(0.2286) H17C(0.2339) H17D(0.3033) H71C(0.9637)
 H71D(0.9765) H70C(0.994) H70D(0.985) H12A(1.0154) H12B(0.9376) H1AA(1.0607)
 H1AB(1.0347) H32A(0.5252) H32B(0.5016) H31A(0.5235) H31B(0.4504) H30A(0.5559)
 H30B(0.4855)
 Fixed Y: H0AA(0.3296) H0AB(0.3123) H3A(0.3566) H3B(0.3373) H3AA(0.7597)
 H3AB(0.6961) H3CA(0.0298) H4A(0.3237) H4B(0.3894) H5A(0.3868) H5B(0.4016)
 H6A(0.4979) H6B(0.5) H9A(0.5838) H9B(0.5838) H10A(0.693) H10B(0.6807)
 H11A(0.7256) H11B(0.7408) H15A(0.4334) H15B(0.5037) H15C(0.4308) H15D(0.4885)
 H16A(0.4692) H16B(0.4442) H17A(0.5359) H17B(0.5716) H18A(0.6254) H18B(0.5769)
 H18C(0.6255) H18D(0.5556) H19(0.7263) H21(0.6837) H22(0.7702) H23(0.8306)
 H25(0.4321) H26(0.3466) H28(0.2139) H29(0.2976) H35A(0.0205) H35B(0.0889)
 H36A(0.1091) H36B(0.0321) H37A(0.0218) H37B(0.0828) H38A(0.1517) H38B(0.0873)
 H41A(0.4251) H41B(0.39) H42A(0.4452) H42B(0.4011) H43A(0.3581) H43B(0.3641)
 H46A(0.0448) H46B(-0.0029) H47A(-0.0535) H47B(-0.0516) H48A(0.0395) H48B(-
 0.0238) H49A(0.0163) H49B(0.0797) H52(0.2688) H51(0.2638) H55(0.1292)
 H54(0.1341) H56(0.16) H58(0.0338) H59(0.0049) H60(0.0538) H69A(0.4402)
 H69B(0.5048) H69C(0.4788) H69D(0.4487) H70A(0.5033) H70B(0.4917) H71A(0.599)
 H71B(0.5304) H72C(0.6142) H72D(0.6458) H72A(0.5976) H72B(0.6497) H75A(0.2993)
 H75B(0.3087) H76A(0.2857) H76B(0.3298) H77A(0.3778) H77B(0.3824) H78A(0.48)
 H78B(0.4488) H79(0.7126) H81(0.6725) H82(0.7643) H83(0.8348) H85(0.2696)
 H86(0.175) H88(0.2565) H89(0.3449) H90A(0.095) H90B(0.0703) H91A(0.1711)
 H91B(0.0991) H92A(0.1744) H92B(0.1864) H94(0.1948) H95(0.1937) H97(0.0087)
 H98(0.0062) H10C(0.1999) H10D(0.2481) H10E(0.3106) H10F(0.2985) H10G(0.2171)
 H10H(0.2851) H10I(0.2538) H10J(0.1914) H10K(0.178) H10L(0.102) H10M(0.1442)
 H10N(0.0834) H10O(0.171) H10P(0.2162) H11C(0.1773) H11D(0.1048) H11E(-0.1092)
 H11F(-0.0938) H11G(-0.1028) H11H(-0.0953) H11I(-0.1511) H11J(-0.1953) H11K(-
 0.1508) H11L(-0.1978) H11O(-0.0854) H11P(-0.1064) H11M(-0.0922) H11N(-0.0963)
 H117(0.1355) H119(0.0403) H120(0.0797) H16C(0.5028) H16D(0.4768) H17C(0.5826)
 H17D(0.6039) H71C(0.6134) H71D(0.6169) H70C(0.5399) H70D(0.5898) H12A(-0.1562)
 H12B(-0.1912) H1AA(-0.1557) H1AB(-0.1951) H32A(0.127) H32B(0.1893)
 H31A(0.1415) H31B(0.1382) H30A(0.2549) H30B(0.2545)
 Fixed Z: H0AA(0.0431) H0AB(0.0983) H3A(0.7196) H3B(0.7375) H3AA(0.6157)
 H3AB(0.6386) H3CA(0.2044) H4A(0.8194) H4B(0.816) H5A(0.8451) H5B(0.893)
 H6A(0.8679) H6B(0.8614) H9A(0.5694) H9B(0.5272) H10A(0.543) H10B(0.5351)
 H11A(0.7015) H11B(0.6498) H15A(0.5622) H15B(0.5429) H15C(0.5757) H15D(0.5373)
 H16A(0.5683) H16B(0.6267) H17A(0.6575) H17B(0.6057) H18A(0.6706) H18B(0.7176)
 H18C(0.6932) H18D(0.7053) H19(0.8411) H21(0.8279) H22(0.9043) H23(0.9451)
 H25(0.471) H26(0.3955) H28(0.5031) H29(0.5789) H35A(-0.0848) H35B(-0.1024)
 H36A(-0.1417) H36B(-0.1545) H37A(-0.0957) H37B(-0.1276) H38A(-0.0459) H38B(-
 0.0179) H41A(0.1038) H41B(0.1607) H42A(0.1338) H42B(0.0718) H43A(0.1237)
 H43B(0.1805) H46A(0.2101) H46B(0.1501) H47A(0.1855) H47B(0.2348) H48A(0.2859)
 H48B(0.2799) H49A(0.2147) H49B(0.2599) H52(0.288) H51(0.2331) H55(0.1126)
 H54(0.1675) H56(0.0784) H58(-0.0516) H59(-0.0778) H60(-0.0295) H69A(1.0158)
 H69B(0.9964) H69C(0.9872) H69D(1.04) H70A(1.0915) H70B(1.1037) H71A(1.1386)
 H71B(1.1199) H72C(1.1099) H72D(1.0662) H72A(1.1156) H72B(1.0721) H75A(0.9412)
 H75B(1.0074) H76A(1.0151) H76B(0.9661) H77A(1.0622) H77B(1.079) H78A(1.0562)
 H78B(0.9979) H79(0.9395) H81(1.1034) H82(1.1312) H83(1.0653) H85(0.8364)
 H86(0.7873) H88(0.8182) H89(0.8703) H90A(0.7528) H90B(0.7157) H91A(0.689)
 H91B(0.6552) H92A(0.6002) H92B(0.6512) H94(0.493) H95(0.5543) H97(0.5755)
 H98(0.5045) H10C(0.1992) H10D(0.2394) H10E(0.2802) H10F(0.2122) H10G(0.2281)
 H10H(0.2633) H10I(0.3508) H10J(0.3172) H10K(0.4407) H10L(0.4261) H10M(0.5272)
 H10N(0.5209) H10O(0.5913) H10P(0.5401) H11C(0.5511) H11D(0.5522) H11E(0.287)
 H11F(0.2322) H11G(0.2354) H11H(0.2683) H11I(0.2586) H11J(0.2734) H11K(0.275)
 H11L(0.3246) H11O(0.3639) H11P(0.4012) H11M(0.405) H11N(0.342) H117(0.1694)
 H119(0.2751) H120(0.1216) H16C(0.5543) H16D(0.6162) H17C(0.6285) H17D(0.595)
 H71C(1.1302) H71D(1.062) H70C(1.091) H70D(1.0481) H12A(0.3706) H12B(0.3452)
 H1AA(0.3373) H1AB(0.2733) H32A(0.2393) H32B(0.2339) H31A(0.3397) H31B(0.3128)
 H30A(0.3626) H30B(0.3315)
;
_shelx_res_checksum              86266
_shelx_hkl_checksum              45863
_shelx_fab_checksum              25564
_olex2_submission_special_instructions 'No special instructions were received'