Kinetic selection of Pd<sub>4</sub>L<sub>2</sub> metallocyclic and Pd<sub>6</sub>L<sub>3</sub> trigonal prismatic assemblies.
O'Connor, Helen M; Coletta, Marco; Etcheverry-Berríos, Alvaro; Nichol, Gary S.; Brechin, Euan K.; Lusby, Paul J.; Chemical communications (Cambridge, England) 56 (2020) 11799–11802; doi:10.1039/d0cc05311b

data_7127114
_publ_section_title
;
 Kinetic selection of Pd<sub>4</sub>L<sub>2</sub> metallocyclic and
 Pd<sub>6</sub>L<sub>3</sub> trigonal prismatic assemblies.
;
_journal_issue                   79
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11799
_journal_page_last               11802
_journal_paper_doi               10.1039/d0cc05311b
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C264 H210 N12 P12 Pd6), 8(C2 F6 O6 S2)'
_chemical_formula_sum            'C552 H418 F72 N24 O72 P24 Pd12 S24'
_chemical_formula_weight         12696.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-07
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-03 deposited with the CCDC.	2020-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6651(16)
_cell_length_b                   51.156(4)
_cell_length_c                   74.909(6)
_cell_measurement_reflns_used    9572
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      19.717
_cell_measurement_theta_min      2.200
_cell_volume                     71525(10)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            PILATUS_2M_S_N_24_0107_Diamond
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_limit_l_min       -74
_diffrn_reflns_number            319787
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        20.148
_diffrn_reflns_theta_max         20.148
_diffrn_reflns_theta_min         0.772
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  0.4282
_exptl_absorpt_correction_T_min  0.3073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1501 before and 0.0777 after correction.
The Ratio of minimum to maximum transmission is 0.7177.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       needle
_exptl_crystal_F_000             25672
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of acetonitrile and diethyl ether  by vapour diffusion'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.642
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2375
_refine_ls_number_reflns         38942
_refine_ls_number_restraints     3264
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1206P)^2^+64.0788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1863
_reflns_Friedel_coverage         0.980
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                30924
_reflns_number_total             38942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05311b2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7127112--7127114.cif.'
_cod_original_cell_volume        71526(11)
_cod_database_code               7127114
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.889
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(3)
 0.47(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 S551-C551 = S591-C591 = S561-C561 = S541-C541 = S641-C641 = S611-C611 = S601-
 C601 = S571-C571 = S511-C511 = S621-C621 = S501-C501 = S521-C521 = S531-C531 =
 S631-C631 = S651-C651 = S581-C581
 1.8 with sigma of 0.01
 F554-C551 = F552-C551 = F542-C541 = F541-C541 = F593-C591 = F591-C591 = F592-
 C591 = F561-C561 = F562-C561 = F563-C561 = F641-C641 = F642-C641 = F643-C641 =
 F612-C611 = F613-C611 = F611-C611 = F601-C601 = F602-C601 = F603-C601 = F573-
 C571 = F571-C571 = F572-C571 = F581-C581 = F582-C581 = F583-C581 = F653-C651 =
 F651-C651 = F652-C651 = F513-C511 = F512-C511 = F511-C511 = F632-C631 = F633-
 C631 = F631-C631 = F532-C531 = F531-C531 = F533-C531 = F523-C521 = F521-C521 =
 F522-C521 = F623-C621 = F622-C621 = F621-C621 = F501-C501 = F502-C501 = F503-
 C501
 1.33 with sigma of 0.01
 S551-O552 = S551-O553 = S551-O551 = S591-O591 = S591-O593 = S591-O592 = S541-
 O543 = S541-O542 = S541-O541 = S561-O563 = S561-O562 = S561-O561 = S641-O643 =
 S641-O642 = S611-O611 = S611-O612 = S621-O621 = S621-O623 = S621-O622 = S511-
 O512 = S511-O513 = S571-O572 = S571-O571 = S571-O573 = S601-O603 = S601-O602 =
 S601-O601 = S651-O652 = S651-O653 = S651-O651 = S581-O583 = S581-O582 = S581-
 O581 = S531-O532 = S531-O533 = S531-O531 = S631-O631 = S631-O632 = S501-O503 =
 S501-O502 = S501-O501 = S521-O522 = S521-O521
 1.43 with sigma of 0.01
 C311-C310 = C305-C304 = C329-C328 = C323-C322 = C287-C286 = C293-C292 = C88-
 C87 = C94-C93 = C124-C123 = C130-C129 = C106-C105 = C112-C111
 1.19 with sigma of 0.01
 F582-F583
 2.13 with sigma of 0.04
 F563-F562
 2.13 with sigma of 0.04
 F621-F622
 2.41 with sigma of 0.04
 O501-O502
 2.41 with sigma of 0.04
 F542-F541
 2.13 with sigma of 0.04
 O501-O503
 2.41 with sigma of 0.04
 F593-F592
 2.13 with sigma of 0.04
 F602-F601
 2.13 with sigma of 0.04
 O512-O513
 2.41 with sigma of 0.04
 F632-F633
 2.41 with sigma of 0.04
 O522-O521
 2.41 with sigma of 0.04
 O502-O503
 2.41 with sigma of 0.04
 O533-O532
 2.41 with sigma of 0.04
 F532-F533
 2.13 with sigma of 0.04
 O532-O531
 2.41 with sigma of 0.04
 F562-F561
 2.13 with sigma of 0.04
 O542-O543
 2.41 with sigma of 0.04
 F573-F571
 2.13 with sigma of 0.04
 O543-O541
 2.41 with sigma of 0.04
 F581-F582
 2.13 with sigma of 0.04
 O541-O542
 2.41 with sigma of 0.04
 F601-F603
 2.13 with sigma of 0.04
 O552-O551
 2.41 with sigma of 0.04
 F613-F612
 2.13 with sigma of 0.04
 O551-O553
 2.41 with sigma of 0.04
 F623-F621
 2.41 with sigma of 0.04
 O553-O552
 2.41 with sigma of 0.04
 F641-F642
 2.41 with sigma of 0.04
 O563-O562
 2.41 with sigma of 0.04
 O531-O533
 2.41 with sigma of 0.04
 F643-F641
 2.41 with sigma of 0.04
 O561-O563
 2.41 with sigma of 0.04
 O572-O571
 2.41 with sigma of 0.04
 O571-O573
 2.41 with sigma of 0.04
 F531-F532
 2.13 with sigma of 0.04
 O573-O572
 2.41 with sigma of 0.04
 F533-F531
 2.13 with sigma of 0.04
 O583-O582
 2.41 with sigma of 0.04
 F554-F552
 2.13 with sigma of 0.04
 O582-O581
 2.41 with sigma of 0.04
 F561-F563
 2.13 with sigma of 0.04
 O581-O583
 2.41 with sigma of 0.04
 F572-F573
 2.13 with sigma of 0.04
 O591-O593
 2.41 with sigma of 0.04
 F571-F572
 2.13 with sigma of 0.04
 O593-O592
 2.41 with sigma of 0.04
 F581-F583
 2.13 with sigma of 0.04
 O592-O591
 2.41 with sigma of 0.04
 F591-F593
 2.13 with sigma of 0.04
 O603-O601
 2.41 with sigma of 0.04
 F592-F591
 2.13 with sigma of 0.04
 O601-O602
 2.41 with sigma of 0.04
 F603-F602
 2.13 with sigma of 0.04
 O602-O603
 2.41 with sigma of 0.04
 F611-F613
 2.13 with sigma of 0.04
 O611-O612
 2.41 with sigma of 0.04
 F612-F611
 2.13 with sigma of 0.04
 O621-O622
 2.41 with sigma of 0.04
 F622-F623
 2.41 with sigma of 0.04
 O622-O623
 2.41 with sigma of 0.04
 F631-F632
 2.41 with sigma of 0.04
 O623-O621
 2.41 with sigma of 0.04
 F633-F631
 2.41 with sigma of 0.04
 O631-O632
 2.41 with sigma of 0.04
 F642-F643
 2.41 with sigma of 0.04
 O643-O642
 2.41 with sigma of 0.04
 O562-O561
 2.41 with sigma of 0.04
 F502-F501
 2.13 with sigma of 0.04
 F502-F503
 2.13 with sigma of 0.04
 F503-F501
 2.13 with sigma of 0.04
 F511-F512
 2.13 with sigma of 0.04
 F512-F513
 2.13 with sigma of 0.04
 F513-F511
 2.13 with sigma of 0.04
 F521-F523
 2.13 with sigma of 0.04
 F523-F522
 2.13 with sigma of 0.04
 F522-F521
 2.13 with sigma of 0.04
 F512-S511
 2.59 with sigma of 0.04
 F613-S611
 2.59 with sigma of 0.04
 F501-S501
 2.59 with sigma of 0.04
 F633-S631
 2.59 with sigma of 0.04
 F522-S521
 2.59 with sigma of 0.04
 F521-S521
 2.59 with sigma of 0.04
 F513-S511
 2.59 with sigma of 0.04
 F523-S521
 2.59 with sigma of 0.04
 F532-S531
 2.59 with sigma of 0.04
 S501-F503
 2.59 with sigma of 0.04
 F561-S561
 2.59 with sigma of 0.04
 F511-S511
 2.59 with sigma of 0.04
 F611-S611
 2.59 with sigma of 0.04
 F632-S631
 2.59 with sigma of 0.04
 F612-S611
 2.59 with sigma of 0.04
 F641-S641
 2.59 with sigma of 0.04
 S501-F502
 2.59 with sigma of 0.04
 F562-S561
 2.59 with sigma of 0.04
 F621-S621
 2.59 with sigma of 0.04
 F563-S561
 2.59 with sigma of 0.04
 F623-S621
 2.59 with sigma of 0.04
 F573-S571
 2.59 with sigma of 0.04
 F531-S531
 2.59 with sigma of 0.04
 F572-S571
 2.59 with sigma of 0.04
 F642-S641
 2.59 with sigma of 0.04
 F571-S571
 2.59 with sigma of 0.04
 F643-S641
 2.59 with sigma of 0.04
 F582-S581
 2.59 with sigma of 0.04
 F533-S531
 2.59 with sigma of 0.04
 F583-S581
 2.59 with sigma of 0.04
 F541-S541
 2.59 with sigma of 0.04
 F581-S581
 2.59 with sigma of 0.04
 F622-S621
 2.59 with sigma of 0.04
 S591-F593
 2.59 with sigma of 0.04
 F542-S541
 2.59 with sigma of 0.04
 S591-F591
 2.59 with sigma of 0.04
 F631-S631
 2.59 with sigma of 0.04
 S591-F592
 2.59 with sigma of 0.04
 F554-S551
 2.59 with sigma of 0.04
 F601-S601
 2.59 with sigma of 0.04
 F552-S551
 2.59 with sigma of 0.04
 F602-S601
 2.59 with sigma of 0.04
 F603-S601
 2.59 with sigma of 0.04
 P4-C30 \\sim P3-C28
 with sigma of 0.02
 C30-C29 \\sim C29-C28
 with sigma of 0.02
 C57-C56 \\sim C56-C55
 with sigma of 0.02
 C3-C2 \\sim C2-C1
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 S631, C631, F631, F633, F632, O631, O632
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S551, C551, F554, F552, O552, O553, O551
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S511, C511, F513, F512, F511, O512, O513
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S591, C591, F592, F591, F593, O593, O591, O592
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S531, C531, F532, F531, F533, O533, O532, O531
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S571, C571, F573, F571, F572, O572, O573, O571
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S611, C611, F612, F611, F613, O612, O611
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S501, O501, O503, O502, C501, F503, F502, F501
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S521, C521, F522, F523, F521, O521, O522
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S541, C541, F542, F541, O541, O542, O543
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S561, C561, F562, F563, F561, O563, O562, O561
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S581, C581, F581, F583, F582, O583, O581, O582
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S601, C601, F602, F601, F603, O602, O603, O601
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S621, C621, F623, F621, F622, O622, O623, O621
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S641, C641, F642, F641, F643, O642, O643
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Pd1, P1, P2, N1, N3, C1, C4, C10, C3, C16, C22, C82, C86, C100, C104, C2, C5,
 C9, C11, C15, C21, C17, C23, C27, C83, C85, C101, C103, C6, C8, C12, C14, C20,
 C18, C24, C26, C84, C87, C102, C105, C7, C13, C19, C25, C88, C106, C89, C107,
 C90, C91, C108, C109, C92, C93, C110, C111, C94, C112, C95, C113, C96, C99,
 C114, C117, C97, N2, C115, N4, C98, Pd2, C116, Pd3, P3, P4, N5, P5, P6, N6,
 C28, C31, C37, C30, C43, C49, C118, C122, C55, C58, C64, C57, C70, C76, C134,
 C135, C29, C32, C36, C42, C38, C44, C48, C54, C50, C119, C121, C56, C63, C59,
 C65, C69, C71, C75, C77, C81, C133, C131, C33, C35, C41, C39, C45, C47, C53,
 C51, C120, C123, C62, C60, C66, C68, C72, C74, C78, C80, C132, C130, C34, C40,
 C46, C52, C124, C61, C67, C73, C79, C129, C125, C127, C126, C128
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Pd51, P51, P52, N51, N53, C201, C204, C210, C203, C216, C222, C281, C285,
 C299, C303, C202, C209, C205, C215, C211, C221, C217, C223, C227, C282, C284,
 C300, C302, C208, C206, C214, C212, C220, C218, C224, C226, C283, C286, C301,
 C304, C207, C213, C219, C225, C287, C305, C288, C306, C289, C290, C307, C308,
 C291, C292, C309, C310, C293, C311, C294, C312, C295, C298, C313, C316, C296,
 N52, C314, N54, C297, Pd52, C315, Pd53, P53, P54, N55, P55, P56, N56, C228,
 C231, C237, C230, C243, C248, C317, C321, C254, C257, C263, C256, C269, C275,
 C333, C334, C229, C232, C236, C242, C238, C244, C196, C253, C249, C318, C320,
 C255, C258, C262, C264, C268, C274, C270, C280, C276, C332, C330, C233, C235,
 C241, C239, C245, C247, C252, C250, C319, C322, C259, C261, C265, C267, C273,
 C271, C279, C277, C331, C329, C234, C240, C246, C251, C323, C260, C266, C272,
 C278, C328, C324, C326, C325, C327
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: F501(0.5) F502(0.5) F503(0.5) O501(0.5) O502(0.5) O503(0.5)
 F511(0.5) F512(0.5) F513(0.5) F521(0.5) F523(0.5) F531(0.5) F532(0.5)
 F533(0.5) O531(0.5) O532(0.5) O533(0.5) O541(0.5) O543(0.5) O552(0.5)
 O553(0.5) S561(0.5) F561(0.5) F562(0.5) F563(0.5) O562(0.5) O563(0.5)
 F571(0.5) F572(0.5) F573(0.5) O571(0.5) O572(0.5) O573(0.5) F581(0.5)
 F582(0.5) F583(0.5) O582(0.5) O583(0.5) C581(0.5) F591(0.5) F593(0.5)
 O591(0.5) O593(0.5) F601(0.5) F602(0.5) O601(0.5) O602(0.5) F612(0.5)
 F613(0.5) F621(0.5) F622(0.5) F623(0.5) O622(0.5) O623(0.5) C621(0.5)
 F631(0.5) F632(0.5) F641(0.5) F643(0.5) F651(0.5) F652(0.5) F653(0.5)
 O653(0.5) C651(0.5)
 Fixed Uiso: C651(0.05)
6.a Everything fixed:
 S501, F501, F502, F503, O501, O502, O503, C501, S511, F511, F512, F513, O512,
 O513, C511, S521, F521, F522, F523, O521, O522, C521, S531, F531, F532, F533,
 O531, O532, O533, C531, S541, F541, F542, O541, O542, O543, C541, S551, F552,
 F554, O551, O552, O553, C551, S561, F561, F562, F563, O561, O562, O563, C561,
 S571, F571, F572, F573, O571, O572, O573, C571, S581, F581, F582, F583, O581,
 O582, O583, C581, S591, F591, F592, F593, O591, O592, O593, C591, S601, F601,
 F602, F603, O601, O602, O603, C601, S611, F611, F612, F613, O611, O612, C611,
 S621, F621, F622, F623, O621, O622, O623, C621, S631, F631, F632, F633, O631,
 O632, C631, S641, F641, F642, F643, O642, O643, C641, S651, F651, F652, F653,
 O651, O652, O653, C651
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C201(H20A,
 H20B), C202(H20C,H20D), C203(H20E,H20F), C228(H22A,H22B), C229(H22C,H22D),
 C230(H23A,H23B), C254(H25A,H25B), C255(H25C,H25D), C256(H25E,H25F)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C21(H21), C20(H20), C19(H19), C18(H18), C17(H17), C23(H23),
  C24(H24), C25(H25), C26(H26), C27(H27), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C42(H42), C41(H41), C40(H40), C39(H39), C38(H38), C44(H44),
  C45(H45), C46(H46), C47(H47), C48(H48), C54(H54), C53(H53), C52(H52),
 C51(H51), C50(H50), C63(H63), C62(H62), C61(H61), C60(H60), C59(H59), C65(H65),
  C66(H66), C67(H67), C68(H68), C69(H69), C71(H71), C72(H72), C73(H73),
 C74(H74), C75(H75), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82),
  C84(H84), C85(H85), C86(H86), C90(H90), C92(H92), C96(H96), C97(H97),
 C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C104(H104), C108(H108),
  C110(H110), C114(H114), C115(H115), C116(H116), C117(H117), C118(H118),
 C119(H119), C120(H120), C122(H122), C126(H126), C128(H128), C132(H132),
 C133(H133), C134(H134), C135(H135), C209(H209), C208(H208), C207(H207),
 C206(H206), C205(H205), C215(H215), C214(H214), C213(H213), C212(H212),
 C221(H221), C220(H220), C219(H219), C218(H218), C217(H217), C223(H223),
 C224(H224), C225(H225), C226(H226), C227(H227), C232(H232), C233(H233),
 C234(H234), C235(H235), C236(H236), C242(H242), C241(H241), C240(H240),
 C239(H239), C238(H238), C244(H244), C245(H245), C246(H246), C247(H247),
 C196(H196), C253(H253), C252(H252), C251(H251), C250(H250), C249(H249),
 C258(H258), C259(H259), C260(H260), C261(H261), C262(H262), C264(H264),
 C265(H265), C266(H266), C267(H267), C268(H268), C274(H274), C273(H273),
 C272(H272), C271(H271), C270(H270), C280(H280), C279(H279), C278(H278),
 C277(H277), C276(H276), C281(H281), C282(H282), C283(H283), C285(H285),
 C289(H289), C291(H291), C295(H295), C296(H296), C297(H297), C298(H298),
 C299(H299), C300(H300), C301(H301), C303(H303), C307(H307), C309(H309),
 C313(H313), C314(H314), C315(H315), C316(H316), C317(H317), C318(H318),
 C319(H319), C321(H321), C325(H325), C327(H327), C331(H331), C332(H332),
 C333(H333), C334(H334)
6.d Fitted hexagon refined as free rotating group:
 C4(C5,C6,C7,C8,C9), C10(C11,C12,C13,C14,C15), C16(C21,C20,C19,C18,C17),
 C22(C23,C24,C25,C26,C27), C31(C32,C33,C34,C35,C36), C37(C42,C41,C40,C39,C38),
 C43(C44,C45,C46,C47,C48), C49(C54,C53,C52,C51,C50), C58(C63,C62,C61,C60,C59),
 C64(C65,C66,C67,C68,C69), C70(C71,C72,C73,C74,C75), C76(C77,C78,C79,C80,C81),
 C204(C209,C208,C207,C206,C205), C210(C215,C214,C213,C212,C211), C216(C221,C220,
 C219,C218,C217), C222(C223,C224,C225,C226,C227), C231(C232,C233,C234,C235,
 C236), C237(C242,C241,C240,C239,C238), C243(C244,C245,C246,C247,C196),
 C248(C253,C252,C251,C250,C249), C257(C258,C259,C260,C261,C262), C263(C264,C265,
 C266,C267,C268), C269(C274,C273,C272,C271,C270), C275(C280,C279,C278,C277,C276)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              87431
_shelx_hkl_checksum              87195
_shelx_fab_checksum              96587
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id HOC1356Et2O
_olex2_submission_special_instructions 'No special instructions were received'