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_1544632
_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         '2(C80 H96 B8 Fe4 N28 O24 Pd), 4(B F4)'
_chemical_formula_sum            'C160 H192 B20 F16 Fe8 N56 O48 Pd2'
_chemical_formula_weight         4847.48
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2016-10-21 deposited with the CCDC.
2016-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.789(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   41.2884(9)
_cell_length_b                   14.0841(4)
_cell_length_c                   54.0058(15)
_cell_measurement_reflns_used    22767
_cell_measurement_temperature    140
_cell_measurement_theta_max      50.6780
_cell_measurement_theta_min      3.9450
_cell_volume                     31115.2(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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      140.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.589
_diffrn_measured_fraction_theta_max 0.987
_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  0.1278
_diffrn_reflns_av_unetI/netI     0.1195
_diffrn_reflns_Laue_measured_fraction_full 0.589
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            144401
_diffrn_reflns_point_group_measured_fraction_full 0.589
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         51.143
_diffrn_reflns_theta_min         3.241
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.396
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.22
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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            'clear light orange'
_exptl_crystal_colour_primary    'clear light orange'
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_description       needle
_exptl_crystal_F_000             10224
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN/DMSO/diethyl ether '
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.053
_refine_diff_density_max         3.383
_refine_diff_density_min         -1.925
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2734
_refine_ls_number_reflns         33180
_refine_ls_number_restraints     647
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.2129
_refine_ls_R_factor_gt           0.1467
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+1400.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2909
_refine_ls_wR_factor_ref         0.3321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18384
_reflns_number_total             33180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04732g2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 1544629--1544635.cif.'
_cod_database_code               1544632
_shelxl_version_number           2014-3
_oxdiff_exptl_absorpt_empirical_full_min 0.488
_oxdiff_exptl_absorpt_empirical_full_max 2.747
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F11-B19
 1.3 with sigma of 0.02
 B19-F10
 1.3 with sigma of 0.02
 F9-B19
 1.3 with sigma of 0.02
 B19-F12
 1.3 with sigma of 0.02
 F14-B17 = F13_$1-B17
 1.3 with sigma of 0.02
 B20-F1 = B20-F2 = B20-F3 = B20-F4
 1.3 with sigma of 0.02
 F16-B17
 1.3 with sigma of 0.02
 F6-B18 = F8-B18 = F5-B18 = F7-B18
 1.3 with sigma of 0.02
 F16-B17 = F13-B17 = F14-B17 = F15-B17
 1.3 with sigma of 0.02
 B21-F17 = B21-F18 = B21-F19 = B21-F20
 1.3 with sigma of 0.02
 F9-F10 \\sim F9-F11 \\sim F9-F12 \\sim F10-F11 \\sim F10-F12 \\sim F11-F12
 with sigma of 0.005
 F13-F14 \\sim F13-F15 \\sim F13-F16 \\sim F14-F15 \\sim F14-F16 \\sim F15-F16
 with sigma of 0.005
 F5-F6 \\sim F5-F7 \\sim F5-F8 \\sim F6-F7 \\sim F6-F8 \\sim F7-F8
 with sigma of 0.005
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F2-F3 \\sim F2-F4 \\sim F3-F4
 with sigma of 0.005
 F17-F18 \\sim F17-F19 \\sim F17-F20 \\sim F18-F19 \\sim F18-F20 \\sim F19-F20
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N3A) \\sim Ueq, Uanis(N6A) \\sim Ueq, Uanis(N12A) \\sim Ueq, Uanis(N14A)
\\sim Ueq, Uanis(N7C) \\sim Ueq, Uanis(N12B) \\sim Ueq, Uanis(N10) \\sim Ueq,
Uanis(N6C) \\sim Ueq, Uanis(N8B) \\sim Ueq, Uanis(N11C) \\sim Ueq, Uanis(N12C)
\\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.005
Uanis(B2) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(B3) \\sim Ueq, Uanis(O1B) \\sim
Ueq, Uanis(O3B) \\sim Ueq, Uanis(O4B) \\sim Ueq, Uanis(O11) \\sim Ueq,
Uanis(N2B) \\sim Ueq, Uanis(N5B) \\sim Ueq, Uanis(N6B) \\sim Ueq, Uanis(N8C)
\\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(O6B) \\sim Ueq, Uanis(C26B) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O12) \\sim Ueq, Uanis(C11C) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(O10)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C8B) \\sim Ueq,
Uanis(C10B) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N1B) \\sim Ueq, Uanis(C39C) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C4) \\sim Ueq, Uanis(O11B) \\sim Ueq, Uanis(B12) \\sim Ueq, Uanis(N11B)
\\sim Ueq, Uanis(C33B) \\sim Ueq, Uanis(O11C) \\sim Ueq, Uanis(N11C) \\sim Ueq,
Uanis(C37C) \\sim Ueq, Uanis(N6C) \\sim Ueq, Uanis(C17C) \\sim Ueq, Uanis(C16C)
\\sim Ueq, Uanis(C15C) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.005
Uanis(C9) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C33A)
\\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(N1C) \\sim Ueq, Uanis(C3C) \\sim Ueq,
Uanis(C6B) \\sim Ueq, Uanis(C7B) \\sim Ueq, Uanis(C7C) \\sim Ueq, Uanis(C21B)
\\sim Ueq, Uanis(C36B) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(N12) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(N5C) \\sim Ueq, Uanis(N4B) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(N9A)
\\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(O5B) \\sim Ueq,
Uanis(O7C) \\sim Ueq, Uanis(O8B) \\sim Ueq, Uanis(O10C) \\sim Ueq, Uanis(N7)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O2B, O6B, B10, C18B, O4B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5B, O5B, B9, O1B, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B4, O11, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4A, B6, O6A, O2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18, B2, C19, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: F13(0.5) F14(0.5) F15(0.5) F16(0.5) B17(0.5) F1(0.5) F2(0.5)
 F3(0.5) B20(0.5) F4(0.5)
 Fixed Uiso: F13(0.14) F14(0.14) F15(0.14) F16(0.14) B17(0.14) F5(0.14)
 F6(0.14) F8(0.14) B18(0.14) F9(0.14) F10(0.14) F11(0.14) F12(0.14) B19(0.14)
 F7(0.14) F1(0.14) F2(0.14) F3(0.14) B20(0.14) F4(0.14) F18(0.14) F17(0.14)
 B21(0.14) F19(0.14) F20(0.14)
6.a Aromatic/amide H refined with riding coordinates:
 C13B(H13B), C13C(H13C), C15B(H15B), C15C(H15C), C16B(H16B), C16C(H16C),
 C17B(H17B), C17C(H17C), C19B(H19B), C19C(H19C), C21B(H21B), C21C(H21C),
 C22B(H22B), C22C(H22C), C23B(H23B), C23C(H23C), C36B(H36B), C36C(H36C),
 C38B(H38B), C38C(H38C), C39B(H39B), C39C(H39C), C40B(H40B), C40C(H40C),
 C13(H13), C13A(H13A), C15(H15), C15A(H15A), C16(H16), C16A(H16A), C17(H17),
 C17A(H17A), C19(H19), C19A(H19A), C21(H21), C21A(H21A), C22(H22), C22A(H22A),
 C23(H23), C23A(H23A), C36(H36), C36A(H36A), C38(H38), C38A(H38A), C39(H39),
 C39A(H39A), C40(H40), C40A(H40A)
6.b Idealised Me refined as rotating group:
 C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C4B(H4BA,H4BB,H4BC), C4C(H4CA,H4CB,
 H4CC), C5B(H5BA,H5BB,H5BC), C5C(H5CA,H5CB,H5CC), C8B(H8BA,H8BB,H8BC), C8C(H8CA,
 H8CB,H8CC), C9B(H9BA,H9BB,H9BC), C9C(H9CA,H9CB,H9CC), C12B(H12A,H12B,H12C),
 C12C(H12D,H12E,H12F), C24B(H24A,H24B,H24C), C24C(H24D,H24E,H24F), C27B(H27A,
 H27B,H27C), C27C(H27D,H27E,H27F), C28B(H28A,H28B,H28C), C28C(H28D,H28E,H28F),
 C31B(H31A,H31B,H31C), C31C(H31D,H31E,H31F), C32B(H32A,H32B,H32C), C32C(H32D,
 H32E,H32F), C35B(H35A,H35B,H35C), C35C(H35D,H35E,H35F), C1(H1A,H1B,H1C),
 C1A(H1AA,H1AB,H1AC), C4(H4A,H4B,H4C), C4A(H4AA,H4AB,H4AC), C5(H5A,H5B,H5C),
 C5A(H5AA,H5AB,H5AC), C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C9(H9A,H9B,H9C),
 C9A(H9AA,H9AB,H9AC), C12(H12G,H12H,H12I), C12A(H12J,H12K,H12L), C24(H24G,H24H,
 H24I), C24A(H24J,H24K,H24L), C27(H27G,H27H,H27I), C27A(H27J,H27K,H27L),
 C28(H28G,H28H,H28I), C28A(H28J,H28K,H28L), C31(H31G,H31H,H31I), C31A(H31J,H31K,
 H31L), C32(H32G,H32H,H32I), C32A(H32J,H32K,H32L), C35(H35G,H35H,H35I),
 C35A(H35J,H35K,H35L)
;
_shelx_res_checksum              62743
_shelx_hkl_checksum              1761
_shelx_fab_checksum              2768
_olex2_submission_special_instructions 'No special instructions were received'