[Ag115S34(SCH2C6H4tBu)47(dpph)6]: synthesis, crystal structure and NMR investigations of a soluble silver chalcogenide nanocluster
Bestgen, Sebastian; Fuhr, Olaf; Breitung, Ben; Kiran Chakravadhanula, Venkata Sei; Guthausen, Gisela; Hennrich, Frank; Yu, Wen; Kappes, Manfred M.; Roesky, Peter W.; Fenske, Dieter; Chem. Sci. 8 (2017) 2235–; doi:10.1039/C6SC04578B

data_1544788
_publ_section_title
;
 [Ag115S34(SCH2C6H4tBu)47(dpph)6]: synthesis, crystal structure and NMR
 investigations of a soluble silver chalcogenide nanocluster
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              2235
_journal_paper_doi               10.1039/C6SC04578B
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C697 H897 Ag115 P12 S81'
_chemical_formula_sum            'C697 H897 Ag115 P12 S81'
_chemical_formula_weight         24648.64
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2016-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-30 deposited with the CCDC.
2016-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                86.3790(10)
_cell_angle_beta                 75.6370(10)
_cell_angle_gamma                74.1640(10)
_cell_formula_units_Z            2
_cell_length_a                   29.4745(4)
_cell_length_b                   35.8121(5)
_cell_length_c                   48.4263(7)
_cell_measurement_reflns_used    310660
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      58.24
_cell_measurement_theta_min      1.59
_cell_volume                     47638.4(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.679
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '2.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1068
_diffrn_reflns_av_unetI/netI     0.1127
_diffrn_reflns_Laue_measured_fraction_full 0.679
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            294599
_diffrn_reflns_point_group_measured_fraction_full 0.679
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         55.349
_diffrn_reflns_theta_min         1.587
_diffrn_source                   'Cu Genix 3D'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            Cu
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    20.594
_exptl_absorpt_correction_T_max  0.3470
_exptl_absorpt_correction_T_min  0.0399
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       block
_exptl_crystal_F_000             23920
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         5.630
_refine_diff_density_min         -3.471
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4246
_refine_ls_number_reflns         117059
_refine_ls_number_restraints     326
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.1860
_refine_ls_R_factor_gt           0.1217
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3358
_refine_ls_wR_factor_ref         0.3793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                55411
_reflns_number_total             117059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04578b2.cif
_cod_data_source_block           agsdpp6_sq
_cod_depositor_comments          'Adding full bibliography for 1544788.cif.'
_cod_database_code               1544788
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(C) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C499-C496 = C497-C496 = C498-C496 = C496-C493
 1.54 with sigma of 0.02
 C497-C498 = C498-C499 = C510-C508
 2.51 with sigma of 0.02
 C504-C510 = C504-C509 = C504-C508 = C509-C508 = C509-C510
 2.51 with sigma of 0.02
 C398-C399 = C398-C394 = C398-C400 = C400-C399
 2.51 with sigma of 0.02
 C397-C394 = C399-C397 = C398-C397 = C400-C397
 1.54 with sigma of 0.02
 C661-C658 = C664-C661 = C663-C661 = C662-C661
 1.54 with sigma of 0.02
 C664-C663 = C663-C662 = C664-C662 = C658-C664
 2.51 with sigma of 0.02
 C631-C628 = C630-C628 = C629-C628 = C628-C625
 1.54 with sigma of 0.02
 C533-C534 = C551-C548 = C554-C551 = C553-C551 = C552-C551
 1.54 with sigma of 0.02
 C464-C463 = C463-C460 = C466-C463 = C465-C463 = C441-C438
 1.54 with sigma of 0.02
 C552-C548 = C548-C554 = C548-C553 = C553-C552
 2.51 with sigma of 0.02
 C595-C592 = C596-C595 = C598-C595 = C597-C595
 1.54 with sigma of 0.02
 C595-C593
 2.54 with sigma of 0.02
 C592-C598 = C592-C597 = C592-C596 = C596-C598
 2.51 with sigma of 0.02
 C597-C596 = C598-C597 = C453-C449
 2.51 with sigma of 0.02
 C455-C454 = C454-C453 = C455-C453 = C455-C449 = C454-C449
 2.51 with sigma of 0.02
 S33-C533
 1.9 with sigma of 0.04
 C257-C251 = C257-C256 = C257-C255 = C256-C255
 2.51 with sigma of 0.02
 C254-C251 = C255-C254 = C257-C254 = C256-C254
 1.54 with sigma of 0.02
 C521-C518 = C519-C518 = C520-C518 = C518-C515
 1.54 with sigma of 0.02
 C521-C519 = C520-C521 = C520-C519 = C515-C520 = C515-C521 = C515-C519
 2.51 with sigma of 0.02
 C529-C526 = C532-C529 = C531-C529 = C530-C529
 1.54 with sigma of 0.02
 C531-C530
 2.51 with sigma of 0.02
 C530-C532
 2.51 with sigma of 0.02
 C531-C532
 2.51 with sigma of 0.02
 C526-C532
 2.51 with sigma of 0.02
 C531-C526
 2.51 with sigma of 0.02
 C530-C526
 2.51 with sigma of 0.02
 C487-C488 = C487-C486 = C486-C488
 2.51 with sigma of 0.02
 C488-C485 = C486-C485 = C487-C485
 1.54 with sigma of 0.02
 C658-C663 = C658-C662 = C697-C695 = C400-C394
 2.51 with sigma of 0.02
 C563-C562 = C565-C562 = C564-C562
 1.54 with sigma of 0.02
 C455-C452 = C454-C452 = C453-C452 = C452-C449 = C563-C562
 1.54 with sigma of 0.02
 C565-C559 = C564-C559 = C563-C559 = C564-C565 = C563-C564 = C563-C565
 2.51 with sigma of 0.02
 C534-C533
 1.54 with sigma of 0.02
 C539-C533
 2.54 with sigma of 0.02
 C535-C533
 2.54 with sigma of 0.02
 C672-C669 = C674-C672 = C675-C672 = C673-C672
 1.54 with sigma of 0.02
 C675-C673 = C669-C674
 2.51 with sigma of 0.02
 C669-C673 = C669-C675 = C669-C674 = C675-C673 = C675-C674 = C674-C673
 2.51 with sigma of 0.02
 C683-C681
 2.54 with sigma of 0.02
 C684-C685 = C684-C686 = C684-C680
 2.51 with sigma of 0.02
 C683-C680 = C684-C683 = C685-C683 = C683-C686
 1.54 with sigma of 0.02
 C474-C471 = C476-C474 = C475-C474 = C477-C474
 1.54 with sigma of 0.02
 C476-C475 = C477-C475 = C477-C476 = C499-C497
 2.51 with sigma of 0.02
 C477-C471
 2.51 with sigma of 0.02
 C378-C375
 1.54 with sigma of 0.02
 C405-C408 = C411-C408 = C409-C408 = C408-C410 = C512-C511
 1.54 with sigma of 0.02
 C410-C409 = C411-C409
 2.51 with sigma of 0.02
 C411-C410 = C405-C411 = C405-C409 = C405-C410
 2.51 with sigma of 0.02
 C552-C554 = C554-C553 = C574-C576 = C575-C574 = C575-C576
 2.51 with sigma of 0.02
 C573-C570 = C575-C573 = C576-C573 = C574-C573
 1.54 with sigma of 0.02
 C378-C377
 2.51 with sigma of 0.02
 C507-C504 = C510-C507 = C508-C507 = C509-C507
 1.54 with sigma of 0.02
 C641-C639 = C642-C639 = C584-C581 = C585-C584 = C586-C584 = C587-C584
 1.54 with sigma of 0.02
 C639-C640 = C642-C639 = C641-C639 = C639-C636 = C562-C559 = C639-C636
 1.54 with sigma of 0.02
 C193-S2 = S43-C644
 2.74 with sigma of 0.02
 C652-C647 = C651-C652 = C653-C651 = C651-C647 = C653-C647
 2.51 with sigma of 0.02
 C650-C647 = C652-C650 = C653-C650 = C650-C651 = C665-C666
 1.54 with sigma of 0.02
 C232-C233
 1.54 with sigma of 0.02
 C694-C695
 1.54 with sigma of 0.02
 C287-C289
 1.54 with sigma of 0.02
 C419-C421
 1.54 with sigma of 0.02
 C366-C364
 1.54 with sigma of 0.02
 C603-C606
 1.54 with sigma of 0.02
 C606-C609
 1.54 with sigma of 0.02
 C561-C560
 1.39 with sigma of 0.02
 C557-C558
 1.39 with sigma of 0.02
 C560-C559
 1.39 with sigma of 0.02
 C559-C558
 1.39 with sigma of 0.02
 C430-C433
 1.54 with sigma of 0.02
 C500-C501
 1.54 with sigma of 0.02
 C386-C389
 1.54 with sigma of 0.02
 C617-C620
 1.54 with sigma of 0.02
 C618-C617
 1.54 with sigma of 0.02
 C617-C619
 1.54 with sigma of 0.02
 C569-C570
 1.39 with sigma of 0.02
 C547-C548
 1.39 with sigma of 0.02
 C633-C638
 1.39 with sigma of 0.02
 C638-C637
 1.39 with sigma of 0.02
 C484-C483 = C483-C482
 1.39 with sigma of 0.02
 C485-C482
 1.54 with sigma of 0.02
 C540-C537 = C541-C540 = C542-C540 = C543-C540
 1.54 with sigma of 0.02
 C537-C543 = C543-C541 = C542-C541 = C542-C543
 2.51 with sigma of 0.02
 C542-C537 = C541-C537 = C685-C686 = C685-C680 = C686-C680
 2.51 with sigma of 0.02
3. Restrained planarity
 C533, C537, C536, C535, C534, C539, C538, C540
 with sigma of 0.1
 C676, C677, C679, C680, C681, C683
 with sigma of 0.1
 C643, C644, C645, C646, C647, C648, C649, C650
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(S20) \\sim Ueq, Uanis(S28) \\sim Ueq, Uanis(S47) \\sim Ueq, Uanis(S63)
\\sim Ueq, Uanis(S79) \\sim Ueq, Uanis(S80) \\sim Ueq, Uanis(P3) \\sim Ueq:
with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(A112) \\sim Ueq, Uanis(A9) \\sim Ueq, Uanis(A11) \\sim Ueq, Uanis(A17)
\\sim Ueq, Uanis(A18) \\sim Ueq, Uanis(A32) \\sim Ueq: with sigma of 0.05 and
sigma for terminal atoms of 0.1
Uiso(C661) = Uiso(C664) = Uiso(C663) = Uiso(C662)
Uiso(C669) = Uiso(C672) = Uiso(C675) = Uiso(C674) = Uiso(C673)
Uiso(C655) = Uiso(C660) = Uiso(C657) = Uiso(C656) = Uiso(C659) = Uiso(C658) =
Uiso(C661) = Uiso(C664) = Uiso(C663) = Uiso(C662)
Uiso(C685) = Uiso(C684) = Uiso(C683) = Uiso(C686) = Uiso(C680) = Uiso(C679) =
Uiso(C681) = Uiso(C678) = Uiso(C677) = Uiso(C682)
Uiso(C510) = Uiso(C508) = Uiso(C509)
Uiso(C697) = Uiso(C696) = Uiso(C695)
Uiso(C534) = Uiso(C535)
Uiso(C595) = Uiso(C598) = Uiso(C596) = Uiso(C597)
Uiso(C474) = Uiso(C475) = Uiso(C477) = Uiso(C476)
Uiso(C573) = Uiso(C576) = Uiso(C575) = Uiso(C574)
Uiso(C375) = Uiso(C377) = Uiso(C376) = Uiso(C378)
Uiso(C507) = Uiso(C510) = Uiso(C509) = Uiso(C508)
Uiso(C643) = Uiso(C644) = Uiso(C649) = Uiso(C645) = Uiso(C646) = Uiso(C647) =
Uiso(C648) = Uiso(C650) = Uiso(C651) = Uiso(C653) = Uiso(C652)
5. Others
 Fixed Sof: A1(0.5) A8(0.5) A3(0.5) A4(0.5) A5(0.5) A7(0.5) A13(0.5) A14(0.5)
 A113(0.5) A114(0.5) A1A(0.5) A4A(0.5) A5A(0.5) A7A(0.5) A13A(0.5) A13B(0.5)
 A14A(0.5) A14B(0.5) A3B(0.3) A4B(0.4) A13C(0.3) A1B(0.5) A8A(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,
 H17B), C18(H18A,H18B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C73(H73A,H73B), C74(H74A,H74B),
  C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C103(H10A,
 H10B), C104(H10C,H10D), C105(H10E,H10F), C106(H10G,H10H), C107(H10I,H10J),
 C108(H10K,H10L), C133(H13C,H13D), C134(H13E,H13F), C135(H13G,H13H), C136(H13I,
 H13J), C137(H13K,H13L), C138(H13M,H13N), C163(H16C,H16D), C164(H16E,H16F),
 C165(H16G,H16H), C166(H16I,H16J), C167(H16K,H16L), C168(H16M,H16N), C181(H18C,
 H18D), C192(H19G,H19H), C203(H20J,H20K), C214(H21J,H21K), C225(H22J,H22K),
 C236(H23J,H23K), C247(H24J,H24K), C258(H25J,H25K), C269(H26J,H26K), C280(H28A,
 H28B), C291(H29D,H29E), C302(H30G,H30H), C313(H31J,H31K), C324(H32J,H32K),
 C335(H33J,H33K), C346(H34J,H34K), C357(H35J,H35K), C368(H36J,H36K), C379(H37J,
 H37K), C390(H39A,H39B), C401(H40D,H40E), C412(H41G,H41H), C423(H42J,H42K),
 C434(H43L,H43M), C445(H44L,H44M), C456(H45L,H45M), C467(H46L,H46M), C478(H47L,
 H47M), C489(H48L,H48M), C500(H50A,H50B), C511(H51D,H51E), C522(H52G,H52H),
 C533(H53J,H53K), C544(H54J,H54K), C555(H55J,H55K), C566(H56J,H56K), C577(H57J,
 H57K), C588(H58J,H58K), C599(H59J,H59K), C610(H61A,H61B), C621(H62D,H62E),
 C632(H63G,H63H), C643(H64J,H64K), C654(H65J,H65K), C665(H66J,H66K), C676(H67J,
 H67K), C687(H68J,H68K)
6.b Me refined with riding coordinates:
 C189(H18E,H18F,H18G), C190(H19A,H19B,H19C), C191(H19D,H19E,H19F), C200(H20A,
 H20B,H20C), C201(H20D,H20E,H20F), C202(H20G,H20H,H20I), C211(H21A,H21B,H21C),
 C212(H21D,H21E,H21F), C213(H21G,H21H,H21I), C222(H22A,H22B,H22C), C223(H22D,
 H22E,H22F), C224(H22G,H22H,H22I), C233(H23A,H23B,H23C), C234(H23D,H23E,H23F),
 C235(H23G,H23H,H23I), C244(H24A,H24B,H24C), C245(H24D,H24E,H24F), C246(H24G,
 H24H,H24I), C255(H25A,H25B,H25C), C256(H25D,H25E,H25F), C257(H25G,H25H,H25I),
 C266(H26A,H26B,H26C), C267(H26D,H26E,H26F), C268(H26G,H26H,H26I), C277(H27A,
 H27B,H27C), C278(H27D,H27E,H27F), C279(H27G,H27H,H27I), C288(H28C,H28D,H28E),
 C289(H28F,H28G,H28H), C290(H29A,H29B,H29C), C299(H29F,H29G,H29H), C300(H30A,
 H30B,H30C), C301(H30D,H30E,H30F), C310(H31A,H31B,H31C), C311(H31D,H31E,H31F),
 C312(H31G,H31H,H31I), C321(H32A,H32B,H32C), C322(H32D,H32E,H32F), C323(H32G,
 H32H,H32I), C332(H33A,H33B,H33C), C333(H33D,H33E,H33F), C334(H33G,H33H,H33I),
 C343(H34A,H34B,H34C), C344(H34D,H34E,H34F), C345(H34G,H34H,H34I), C354(H35A,
 H35B,H35C), C355(H35D,H35E,H35F), C356(H35G,H35H,H35I), C365(H36A,H36B,H36C),
 C366(H36D,H36E,H36F), C367(H36G,H36H,H36I), C376(H37A,H37B,H37C), C377(H37D,
 H37E,H37F), C378(H37G,H37H,H37I), C387(H38A,H38B,H38C), C388(H38D,H38E,H38F),
 C389(H38G,H38H,H38I), C398(H39C,H39D,H39E), C399(H39F,H39G,H39H), C400(H40A,
 H40B,H40C), C409(H40F,H40G,H40H), C410(H41A,H41B,H41C), C411(H41D,H41E,H41F),
 C420(H42A,H42B,H42C), C421(H42D,H42E,H42F), C422(H42G,H42H,H42I), C431(H43C,
 H43D,H43E), C432(H43F,H43G,H43H), C433(H43I,H43J,H43K), C442(H44C,H44D,H44E),
 C443(H44F,H44G,H44H), C444(H44I,H44J,H44K), C453(H45C,H45D,H45E), C454(H45F,
 H45G,H45H), C455(H45I,H45J,H45K), C464(H46C,H46D,H46E), C465(H46F,H46G,H46H),
 C466(H46I,H46J,H46K), C475(H47C,H47D,H47E), C476(H47F,H47G,H47H), C477(H47I,
 H47J,H47K), C486(H48C,H48D,H48E), C487(H48F,H48G,H48H), C488(H48I,H48J,H48K),
 C497(H49A,H49B,H49C), C498(H49D,H49E,H49F), C499(H49G,H49H,H49I), C508(H50C,
 H50D,H50E), C509(H50F,H50G,H50H), C510(H51A,H51B,H51C), C519(H51F,H51G,H51H),
 C520(H52A,H52B,H52C), C521(H52D,H52E,H52F), C530(H53A,H53B,H53C), C531(H53D,
 H53E,H53F), C532(H53G,H53H,H53I), C541(H54A,H54B,H54C), C542(H54D,H54E,H54F),
 C543(H54G,H54H,H54I), C552(H55A,H55B,H55C), C553(H55D,H55E,H55F), C554(H55G,
 H55H,H55I), C563(H56A,H56B,H56C), C564(H56D,H56E,H56F), C565(H56G,H56H,H56I),
 C574(H57A,H57B,H57C), C575(H57D,H57E,H57F), C576(H57G,H57H,H57I), C585(H58A,
 H58B,H58C), C586(H58D,H58E,H58F), C587(H58G,H58H,H58I), C596(H59A,H59B,H59C),
 C597(H59D,H59E,H59F), C598(H59G,H59H,H59I), C607(H60A,H60B,H60C), C608(H60D,
 H60E,H60F), C609(H60G,H60H,H60I), C618(H61C,H61D,H61E), C619(H61F,H61G,H61H),
 C620(H62A,H62B,H62C), C629(H62F,H62G,H62H), C630(H63A,H63B,H63C), C631(H63D,
 H63E,H63F), C640(H64A,H64B,H64C), C641(H64D,H64E,H64F), C642(H64G,H64H,H64I),
 C651(H65A,H65B,H65C), C652(H65D,H65E,H65F), C653(H65G,H65H,H65I), C662(H66A,
 H66B,H66C), C663(H66D,H66E,H66F), C664(H66G,H66H,H66I), C673(H67A,H67B,H67C),
 C674(H67D,H67E,H67F), C675(H67G,H67H,H67I), C684(H68A,H68B,H68C), C685(H68D,
 H68E,H68F), C686(H68G,H68H,H68I), C695(H69A,H69B,H69C), C696(H69D,H69E,H69F),
 C697(H69G,H69H,H69I)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C50(H50), C51(H51),
  C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59),
 C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C69(H69),
  C70(H70), C71(H71), C72(H72), C80(H80), C81(H81), C82(H82), C83(H83),
 C84(H84), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93),
  C94(H94), C95(H95), C96(H96), C98(H98), C99(H99), C100(H100), C101(H101),
 C102(H102), C110(H110), C111(H111), C112(H112), C113(H113), C114(H114),
 C116(H116), C117(H117), C118(H118), C119(H119), C120(H120), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C128(H128), C129(H129),
 C130(H130), C131(H131), C132(H132), C140(H140), C141(H141), C142(H142),
 C143(H143), C144(H144), C146(H146), C147(H147), C148(H148), C149(H149),
 C150(H150), C152(H152), C153(H153), C154(H154), C155(H155), C156(H156),
 C158(H158), C159(H159), C160(H160), C161(H161), C162(H162), C170(H170),
 C171(H171), C172(H172), C173(H173), C174(H174), C176(H176), C177(H177),
 C178(H178), C179(H179), C180(H180), C183(H183), C184(H184), C186(H186),
 C187(H187), C194(H194), C195(H195), C197(H197), C198(H198), C205(H205),
 C206(H206), C208(H208), C209(H209), C216(H216), C217(H217), C219(H219),
 C220(H220), C227(H227), C228(H228), C230(H230), C231(H231), C238(H238),
 C239(H239), C241(H241), C242(H242), C249(H249), C250(H250), C252(H252),
 C253(H253), C260(H260), C261(H261), C263(H263), C264(H264), C271(H271),
 C272(H272), C274(H274), C275(H275), C282(H282), C283(H283), C285(H285),
 C286(H286), C293(H293), C294(H294), C296(H296), C297(H297), C304(H304),
 C305(H305), C307(H307), C308(H308), C315(H315), C316(H316), C318(H318),
 C319(H319), C326(H326), C327(H327), C329(H329), C330(H330), C337(H337),
 C338(H338), C340(H340), C341(H341), C348(H348), C349(H349), C351(H351),
 C352(H352), C359(H359), C360(H360), C362(H362), C363(H363), C370(H370),
 C371(H371), C373(H373), C374(H374), C381(H381), C382(H382), C384(H384),
 C385(H385), C392(H392), C393(H393), C395(H395), C396(H396), C407(H407),
 C406(H406), C404(H404), C403(H403), C414(H414), C415(H415), C417(H417),
 C418(H418), C425(H425), C426(H426), C428(H428), C429(H429), C436(H436),
 C437(H437), C439(H439), C440(H440), C447(H447), C448(H448), C450(H450),
 C451(H451), C458(H458), C459(H459), C461(H461), C462(H462), C469(H469),
 C470(H470), C472(H472), C473(H473), C480(H480), C481(H481), C483(H483),
 C484(H484), C491(H491), C492(H492), C494(H494), C495(H495), C502(H502),
 C503(H503), C505(H505), C506(H506), C513(H513), C514(H514), C516(H516),
 C517(H517), C524(H524), C525(H525), C527(H527), C528(H528), C536(H536),
 C535(H535), C539(H539), C538(H538), C546(H546), C547(H547), C549(H549),
 C550(H550), C557(H557), C558(H558), C560(H560), C561(H561), C568(H568),
 C569(H569), C571(H571), C572(H572), C579(H579), C580(H580), C582(H582),
 C583(H583), C590(H590), C591(H591), C593(H593), C594(H594), C601(H601),
 C602(H602), C604(H604), C605(H605), C612(H612), C613(H613), C615(H615),
 C616(H616), C623(H623), C624(H624), C626(H626), C627(H627), C634(H634),
 C635(H635), C637(H637), C638(H638), C645(H645), C646(H646), C648(H648),
 C649(H649), C660(H660), C659(H659), C657(H657), C656(H656), C667(H667),
 C668(H668), C670(H670), C671(H671), C678(H678), C679(H679), C681(H681),
 C682(H682), C689(H689), C690(H690), C692(H692), C693(H693)
6.d Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C7(C8,C9,C10,C11,C12), C19(C20,C21,C22,C23,C24), C25(C26,
 C27,C28,C29,C30), C31(C32,C33,C34,C35,C36), C37(C38,C39,C40,C41,C42), C49(C50,
 C51,C52,C53,C54), C55(C56,C57,C58,C59,C60), C61(C62,C63,C64,C65,C66), C67(C68,
 C69,C70,C71,C72), C79(C80,C81,C82,C83,C84), C85(C86,C87,C88,C89,C90), C91(C92,
 C93,C94,C95,C96), C97(C98,C99,C100,C101,C102), C109(C110,C111,C112,C113,C114),
 C115(C116,C117,C118,C119,C120), C121(C122,C123,C124,C125,C126), C127(C128,C129,
 C130,C131,C132), C139(C140,C141,C142,C143,C144), C145(C146,C147,C148,C149,
 C150), C151(C152,C153,C154,C155,C156), C157(C158,C159,C160,C161,C162),
 C169(C170,C171,C172,C173,C174), C175(C176,C177,C178,C179,C180), C402(C407,C406,
 C405,C404,C403), C537(C536,C535,C534,C539,C538), C589(C590,C591,C592,C593,
 C594), C644(C645,C646,C647,C648,C649), C655(C660,C659,C658,C657,C656),
 C666(C667,C668,C669,C670,C671), C677(C678,C679,C680,C681,C682)
;
_shelx_res_checksum              76696
_shelx_fab_checksum              60809
_olex2_submission_special_instructions 'No special instructions were received'