Synthesis and molecular structure of a spheroidal binary nanoscale copper sulfide cluster.
Bestgen, Sebastian; Fuhr, Olaf; Roesky, Peter W.; Fenske, Dieter; Dalton transactions (Cambridge, England : 2003) 45 (2016) 14907–14910; doi:10.1039/c6dt03311c

data_7040585
_publ_section_title
;
 Synthesis and molecular structure of a spheroidal binary nanoscale copper
 sulfide cluster.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14907
_journal_page_last               14910
_journal_paper_doi               10.1039/c6dt03311c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C452 H540 Cu52 P8 S40, 10(C7 H16)'
_chemical_formula_sum            'C522 H700 Cu52 P8 S40'
_chemical_formula_weight         11809.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-17 deposited with the CCDC.
2016-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.6740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   41.0006(8)
_cell_length_b                   31.9188(4)
_cell_length_c                   45.9429(9)
_cell_measurement_reflns_used    95727
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      60.29
_cell_measurement_theta_min      2.35
_cell_volume                     55065.2(17)
_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 0.802
_diffrn_measured_fraction_theta_max 0.969
_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  'secondary plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_unetI/netI     0.1031
_diffrn_reflns_Laue_measured_fraction_full 0.802
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            147112
_diffrn_reflns_point_group_measured_fraction_full 0.802
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         60.303
_diffrn_reflns_theta_min         2.445
_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    4.080
_exptl_absorpt_correction_T_max  0.7784
_exptl_absorpt_correction_T_min  0.5930
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             24400
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.804
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2657
_refine_ls_number_reflns         39955
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      0.808
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20446
_reflns_number_total             39955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03311c2.cif
_cod_data_source_block           cu52
_cod_depositor_comments
;Adding full bibliography for 7040585.cif.

 Adding full bibliography for 7040585.cif.
;
_cod_database_code               7040585
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C97A-C96
 1.54 with sigma of 0.02
 C93-C97A
 2.51 with sigma of 0.02
 C98A-C97A
 2.51 with sigma of 0.02
 C98A-C96
 1.54 with sigma of 0.02
 C235-C234 = C236-C235 = C237-C236 = C238-C237 = C239-C238 = C240-C239
 1.54 with sigma of 0.02
 C234-C236 = C235-C237 = C236-C238 = C237-C239 = C238-C240
 2.51 with sigma of 0.02
 C99A-C97A
 2.51 with sigma of 0.02
 C256-C255 = C257-C256 = C258-C257 = C259-C258 = C260-C259 = C261-C260
 1.54 with sigma of 0.02
 C255-C257 = C256-C258 = C257-C259 = C258-C260 = C259-C261
 2.51 with sigma of 0.02
 C119-C121 = C121-C120 = C120-C119
 2.51 with sigma of 0.02
 C254-C253 = C253-C252 = C251-C252 = C251-C250 = C249-C250 = C249-C248
 1.54 with sigma of 0.02
 C248-C250 = C249-C251 = C250-C252 = C251-C253 = C252-C254
 2.51 with sigma of 0.02
 C266-C268 = C262-C264 = C263-C265 = C264-C266
 2.51 with sigma of 0.02
 C263-C262 = C264-C263 = C265-C264 = C266-C265 = C267-C266 = C268-C267
 1.54 with sigma of 0.02
 C65B-C64B
 1.54 with sigma of 0.02
 C97-C96
 1.54 with sigma of 0.02
 C229-C227
 2.51 with sigma of 0.02
 H15H-H22D_$1
 2.2 with sigma of 0.02
 C69B-C68B = C68B-C66B = C66B-C65B = C64B-C63B = C63B-C62B
 1.54 with sigma of 0.02
 C69B-C66B = C68B-C65B = C66B-C64B = C65B-C63B = C64B-C62B
 2.51 with sigma of 0.02
 C229-C228 = C230-C229 = C231-C230 = C232-C231 = C233-C232
 1.54 with sigma of 0.02
 C233-C231 = C233-C231 = C232-C230 = C231-C229 = C230-C228
 2.51 with sigma of 0.02
 C228-C227
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C234 \\sim C235 \\sim C236 \\sim C237 \\sim C238 \\sim C239 \\sim C240: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C255 \\sim C256 \\sim C257 \\sim C258 \\sim C259 \\sim C260 \\sim C261: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C248 \\sim C249 \\sim C250 \\sim C251 \\sim C252 \\sim C253 \\sim C254: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C262 \\sim C263 \\sim C264 \\sim C265 \\sim C266 \\sim C267 \\sim C268: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C68B \\sim C65B \\sim C63B \\sim C69B \\sim C66B \\sim C64B \\sim C62B: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C227 \\sim C228 \\sim C229 \\sim C230 \\sim C231 \\sim C232 \\sim C233: within
1.7A with sigma of 0.03 and sigma for terminal atoms of 0.06
4. Others
 Fixed Sof: C31(0.6) H31A(0.6) H31B(0.6) H31C(0.6) C32(0.6) H32A(0.6)
 H32B(0.6) H32C(0.6) C33(0.6) H33A(0.6) H33B(0.6) H33C(0.6) C42(0.5) H42A(0.5)
 H42B(0.5) H42C(0.5) C42A(0.5) H42D(0.5) H42E(0.5) H42F(0.5) C43(0.5) H43A(0.5)
 H43B(0.5) H43C(0.5) C43A(0.5) H43D(0.5) H43E(0.5) H43F(0.5) C44A(0.5)
 H44A(0.5) H44B(0.5) H44C(0.5) C44(0.5) H44D(0.5) H44E(0.5) H44F(0.5) C64(0.65)
 H64A(0.65) H64B(0.65) H64C(0.65) C65(0.65) H65A(0.65) H65B(0.65) H65C(0.65)
 C66(0.65) H66A(0.65) H66B(0.65) H66C(0.65) C97(0.7) H97A(0.7) H97B(0.7)
 H97C(0.7) C98(0.7) H98A(0.7) H98B(0.7) H98C(0.7) C99(0.7) H99A(0.7) H99B(0.7)
 H99C(0.7) C99A(0.3) H99D(0.3) H99E(0.3) H99F(0.3) C97A(0.3) H97D(0.3)
 H97E(0.3) H97F(0.3) C98A(0.3) H98D(0.3) H98E(0.3) H98F(0.3) C262(0.3)
 H26F(0.3) H26G(0.3) H26H(0.3) C263(0.3) H26I(0.3) H26J(0.3) C264(0.3)
 H26K(0.3) H26L(0.3) C265(0.3) H26M(0.3) H26N(0.3) C266(0.3) H26O(0.3)
 H26P(0.3) C267(0.3) H26Q(0.3) H26R(0.3) C268(0.3) H26S(0.3) H26T(0.3)
 H26U(0.3) C32A(0.4) H32D(0.4) H32E(0.4) H32F(0.4) C33A(0.4) H33D(0.4)
 H33E(0.4) H33F(0.4) C31A(0.4) H31D(0.4) H31E(0.4) H31F(0.4) C68B(0.7)
 H68A(0.7) H68B(0.7) C65B(0.7) H65G(0.7) H65H(0.7) C63B(0.7) H63A(0.7)
 H63B(0.7) C69B(0.7) H69A(0.7) H69B(0.7) H69C(0.7) C66B(0.7) H66G(0.7)
 H66H(0.7) C64B(0.7) H64G(0.7) H64H(0.7) C64A(0.35) H64D(0.35) H64E(0.35)
 H64F(0.35) C66A(0.35) H66D(0.35) H66E(0.35) H66F(0.35) C65A(0.35) H65D(0.35)
 H65E(0.35) H65F(0.35) C62B(0.7) H62A(0.7) H62B(0.7) H62C(0.7)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C12(H12A,H12B), C23(H23A,H23B), C34(H34A,H34B), C45(H45A,H45B),
 C56(H56A,H56B), C67(H67A,H67B), C78(H78A,H78B), C89(H89A,H89B), C100(H10D,
 H10E), C111(H11G,H11H), C122(H12I,H12J), C133(H13J,H13K), C144(H14J,H14K),
 C256(H25D,H25E), C257(H25F,H25G), C258(H25H,H25I), C259(H25J,H25K), C260(H26A,
 H26B), C249(H24D,H24E), C250(H25L,H25M), C251(H25N,H25O), C252(H25P,H25Q),
 C253(H25R,H25S), C263(H26I,H26J), C264(H26K,H26L), C265(H26M,H26N), C266(H26O,
 H26P), C267(H26Q,H26R), C235(H23F,H23G), C236(H23H,H23I), C237(H23J,H23K),
 C238(H23L,H23M), C239(H23N,H23O), C228(H22G,H22H), C229(H22I,H22J), C230(H23P,
 H23Q), C231(H23R,H23S), C232(H23T,H23U), C68B(H68A,H68B), C65B(H65G,H65H),
 C63B(H63A,H63B), C66B(H66G,H66H), C64B(H64G,H64H)
5.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C42(H42A,H42B,H42C),
 C42A(H42D,H42E,H42F), C43(H43A,H43B,H43C), C43A(H43D,H43E,H43F), C44A(H44A,
 H44B,H44C), C44(H44D,H44E,H44F), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,
 H77C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C),
 C99A(H99D,H99E,H99F), C108(H10F,H10G,H10H), C109(H10I,H10J,H10K), C110(H11D,
 H11E,H11F), C119(H11I,H11J,H11K), C120(H12C,H12D,H12E), C121(H12F,H12G,H12H),
 C130(H13A,H13B,H13C), C131(H13D,H13E,H13F), C132(H13G,H13H,H13I), C141(H14A,
 H14B,H14C), C142(H14D,H14E,H14F), C143(H14G,H14H,H14I), C152(H15A,H15B,H15C),
 C153(H15D,H15E,H15F), C154(H15G,H15H,H15I), C255(H25A,H25B,H25C), C261(H26C,
 H26D,H26E), C248(H24A,H24B,H24C), C254(H25T,H25U,H25V), C262(H26F,H26G,H26H),
 C268(H26S,H26T,H26U), C234(H23C,H23D,H23E), C240(H24F,H24G,H24H), C227(H22D,
 H22E,H22F), C233(H23V,H23W,H23X), C33A(H33D,H33E,H33F), C31A(H31D,H31E,H31F),
 C69B(H69A,H69B,H69C), C65A(H65D,H65E,H65F)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C14(H14), C15(H15), C17(H17), C18(H18),
 C25(H25), C26(H26), C28(H28), C29(H29), C36(H36), C37(H37), C39(H39), C40(H40),
  C47(H47), C48(H48), C50(H50), C51(H51), C58(H58), C59(H59), C61(H61),
 C62(H62), C69(H69), C70(H70), C72(H72), C73(H73), C80(H80), C81(H81), C83(H83),
  C84(H84), C91(H91), C92(H92), C94(H94), C95(H95), C102(H102), C103(H103),
 C105(H105), C106(H106), C113(H113), C114(H114), C116(H116), C117(H117),
 C124(H124), C125(H125), C127(H127), C128(H128), C135(H135), C136(H136),
 C138(H138), C139(H139), C146(H146), C147(H147), C149(H149), C150(H150),
 C156(H156), C157(H157), C158(H158), C159(H159), C160(H160), C162(H162),
 C163(H163), C164(H164), C165(H165), C166(H166), C168(H168), C169(H169),
 C170(H170), C171(H171), C172(H172), C174(H174), C175(H175), C176(H176),
 C177(H177), C178(H178), C180(H180), C181(H181), C182(H182), C183(H183),
 C184(H184), C186(H186), C187(H187), C188(H188), C189(H189), C190(H190),
 C192(H192), C193(H193), C194(H194), C195(H195), C196(H196), C198(H198),
 C199(H199), C200(H200), C201(H201), C202(H202), C204(H204), C205(H205),
 C206(H206), C207(H207), C208(H208), C210(H210), C211(H211), C212(H212),
 C213(H213), C214(H214), C216(H216), C217(H217), C218(H218), C219(H219),
 C220(H220), C222(H222), C223(H223), C224(H224), C225(H225), C226(H226)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C64(H64A,H64B,
 H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C97(H97A,H97B,H97C), C98(H98A,
 H98B,H98C), C99(H99A,H99B,H99C), C97A(H97D,H97E,H97F), C98A(H98D,H98E,H98F),
 C32A(H32D,H32E,H32F), C64A(H64D,H64E,H64F), C66A(H66D,H66E,H66F), C62B(H62A,
 H62B,H62C)
;
_shelx_res_checksum              22582
_olex2_submission_special_instructions 'No special instructions were received'