Isolable and well-defined butadienyl organocopper(i) aggregates: facile synthesis, structural characterization, and reaction chemistry.
Geng, Weizhi; Wei, Junnian; Zhang, Wen-Xiong; Xi, Zhenfeng; Journal of the American Chemical Society 136 (2014) 610–613; doi:10.1021/ja4114243

data_4120448
_publ_section_title
;
 Isolable and well-defined butadienyl organocopper(i) aggregates: facile
 synthesis, structural characterization, and reaction chemistry.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              610
_journal_page_last               613
_journal_paper_doi               10.1021/ja4114243
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C64 H112 Cu8'
_chemical_formula_sum            'C64 H112 Cu8'
_chemical_formula_weight         1389.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-31
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.19(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.232(3)
_cell_length_b                   16.803(3)
_cell_length_c                   14.491(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3399.5(12)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_unetI/netI     0.1500
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11156
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.20
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.485
_exptl_absorpt_correction_T_max  0.7892
_exptl_absorpt_correction_T_min  0.7069
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         6589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                2856
_reflns_number_total             6589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4114243_si_002.cif
_cod_data_source_block           2a
_cod_original_cell_volume        3399.6(12)
_cod_database_code               4120448
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5A(0.068) H5B(0.068) H6A(0.094) H6B(0.094) H7A(0.167) H7B(0.167)
 H7C(0.167) H8A(0.078) H8B(0.078) H9A(0.143) H9B(0.143) H10A(0.229) H10B(0.229)
 H10C(0.229) H11A(0.118) H11B(0.118) H12A(0.118) H12B(0.118) H13A(0.198)
 H13B(0.198) H13C(0.198) H14A(0.092) H14B(0.092) H15A(0.172) H15B(0.172)
 H16A(0.28) H16B(0.28) H16C(0.28) H21A(0.118) H21B(0.118) H22A(0.191)
 H22B(0.191) H23A(0.272) H23B(0.272) H23C(0.272) H24A(0.094) H24B(0.094)
 H25A(0.187) H25B(0.187) H26A(0.293) H26B(0.293) H26C(0.293) H27A(0.07)
 H27B(0.07) H28A(0.09) H28B(0.09) H29A(0.149) H29B(0.149) H29C(0.149)
 H30A(0.076) H30B(0.076) H31A(0.1) H31B(0.1) H32A(0.145) H32B(0.145) H32C(0.145)
 Fixed X: H5A(0.1645) H5B(0.1615) H6A(0.3169) H6B(0.3152) H7A(0.4072)
 H7B(0.34) H7C(0.3083) H8A(0.1802) H8B(0.2181) H9A(0.0307) H9B(0.0725)
 H10A(0.0595) H10B(0.1686) H10C(0.1226) H11A(0.1711) H11B(0.2048) H12A(0.2663)
 H12B(0.3049) H13A(0.3499) H13B(0.4202) H13C(0.3773) H14A(0.019) H14B(0.0436)
 H15A(-0.1371) H15B(-0.1085) H16A(-0.1132) H16B(-0.1865) H16C(-0.08)
 H21A(0.3797) H21B(0.3521) H22A(0.3455) H22B(0.3198) H23A(0.4796) H23B(0.4816)
 H23C(0.5084) H24A(0.1267) H24B(0.2362) H25A(0.1048) H25B(0.2154) H26A(0.1504)
 H26B(0.144) H26C(0.2438) H27A(0.0171) H27B(-0.0294) H28A(0.1033) H28B(0.1445)
 H29A(0.0648) H29B(-0.0291) H29C(0.0086) H30A(-0.2747) H30B(-0.3486) H31A(-
 0.2829) H31B(-0.3659) H32A(-0.4354) H32B(-0.4593) H32C(-0.3777)
 Fixed Y: H5A(0.14) H5B(0.222) H6A(0.1145) H6B(0.2037) H7A(0.2057) H7B(0.1474)
 H7C(0.2358) H8A(0.2734) H8B(0.2572) H9A(0.2963) H9B(0.2846) H10A(0.4198)
 H10B(0.3989) H10C(0.4114) H11A(0.1106) H11B(0.1903) H12A(0.0423) H12B(0.124)
 H13A(0.0514) H13B(0.0717) H13C(0.1402) H14A(0.1236) H14B(0.0346) H15A(0.0959)
 H15B(0.0062) H16A(0.0953) H16B(0.0285) H16C(0.0063) H21A(-0.1032) H21B(-
 0.1868) H22A(-0.0483) H22B(-0.1327) H23A(-0.0967) H23B(-0.1742) H23C(-0.0919)
 H24A(-0.2649) H24B(-0.2524) H25A(-0.2791) H25B(-0.271) H26A(-0.3948) H26B(-
 0.4038) H26C(-0.3917) H27A(-0.2118) H27B(-0.1305) H28A(-0.1069) H28B(-0.1908)
 H29A(-0.2005) H29B(-0.1665) H29C(-0.2509) H30A(0.0143) H30B(0.0368)
 H31A(0.1474) H31B(0.1619) H32A(0.1374) H32B(0.0642) H32C(0.0579)
 Fixed Z: H5A(0.6566) H5B(0.6043) H6A(0.6068) H6B(0.5748) H7A(0.7167)
 H7B(0.7582) H7C(0.7355) H8A(0.4886) H8B(0.3958) H9A(0.4003) H9B(0.309)
 H10A(0.3359) H10B(0.348) H10C(0.4368) H11A(0.2165) H11B(0.2684) H12A(0.3408)
 H12B(0.3828) H13A(0.2254) H13B(0.3198) H13C(0.2508) H14A(0.1524) H14B(0.1776)
 H15A(0.1644) H15B(0.1753) H16A(0.0106) H16B(0.0235) H16C(0.0212) H21A(0.5614)
 H21B(0.5175) H22A(0.4169) H22B(0.3735) H23A(0.3605) H23B(0.4211) H23C(0.4704)
 H24A(0.3913) H24B(0.4292) H25A(0.5438) H25B(0.5788) H26A(0.4571) H26B(0.5634)
 H26C(0.5348) H27A(0.3198) H27B(0.2821) H28A(0.2064) H28B(0.2402) H29A(0.0852)
 H29B(0.1118) H29C(0.1478) H30A(0.2795) H30B(0.3425) H31A(0.2252) H31B(0.2801)
 H32A(0.1241) H32B(0.1826) H32C(0.1242)
;