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_4120450
_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         'C60 H116 Cl4 Cu8 Li2 N4'
_chemical_formula_sum            'C60 H116 Cl4 Cu8 Li2 N4'
_chemical_formula_weight         1557.57
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 101.894(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3819(5)
_cell_length_b                   12.9444(4)
_cell_length_c                   35.6961(13)
_cell_measurement_temperature    180(2)
_cell_volume                     7407.0(4)
_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      180.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            30976
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.81
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.430
_exptl_absorpt_correction_T_max  0.7932
_exptl_absorpt_correction_T_min  0.7932
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.183
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         14500
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+24.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                10622
_reflns_number_total             14500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4114243_si_002.cif
_cod_data_source_block           3a
_cod_database_code               4120450
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5A(0.048) H5B(0.048) H6A(0.055) H6B(0.055) H7A(0.113) H7B(0.113)
 H7C(0.113) H8A(0.068) H8B(0.068) H9BC(0.12) H9BD(0.12) H9AA(0.12) H9AB(0.12)
 H10A(0.111) H10B(0.111) H10C(0.111) H10D(0.103) H10E(0.103) H10F(0.103)
 H11A(0.052) H11B(0.052) H12A(0.061) H12B(0.061) H13A(0.082) H13B(0.082)
 H13C(0.082) H14A(0.047) H14B(0.047) H15A(0.056) H15B(0.056) H16A(0.1)
 H16B(0.1) H16C(0.1) H21A(0.045) H21B(0.045) H22A(0.056) H22B(0.056)
 H23A(0.098) H23B(0.098) H23C(0.098) H24A(0.055) H24B(0.055) H25A(0.07)
 H25B(0.07) H26A(0.1) H26B(0.1) H26C(0.1) H27A(0.072) H27B(0.072) H28A(0.07)
 H28B(0.07) H29A(0.173) H29B(0.173) H29C(0.173) H30A(0.143) H30B(0.143)
 H31A(0.143) H31B(0.143) H32A(0.179) H32B(0.179) H32C(0.179) H37A(0.055)
 H37B(0.055) H38A(0.084) H38B(0.084) H39A(0.153) H39B(0.153) H39C(0.153)
 H40A(0.061) H40B(0.061) H41A(0.073) H41B(0.073) H42A(0.142) H42B(0.142)
 H42C(0.142) H43A(0.063) H43B(0.063) H44A(0.115) H44B(0.115) H45A(0.142)
 H45B(0.142) H45C(0.142) H46A(0.046) H46B(0.046) H47A(0.061) H47B(0.061)
 H48A(0.108) H48B(0.108) H48C(0.108) H49A(0.134) H49B(0.134) H49C(0.134)
 H50A(0.114) H50B(0.114) H50C(0.114) H51A(0.128) H51B(0.128) H52A(0.126)
 H52B(0.126) H53A(0.162) H53B(0.162) H53C(0.162) H54A(0.193) H54B(0.193)
 H54C(0.193) H55A(0.228) H55B(0.228) H55C(0.228) H56A(0.148) H56B(0.148)
 H56C(0.148) H57A(0.189) H57B(0.189) H58A(0.189) H58B(0.189) H59A(0.177)
 H59B(0.177) H59C(0.177) H60A(0.14) H60B(0.14) H60C(0.14)
 Fixed X: H5A(0.3343) H5B(0.2407) H6A(0.3593) H6B(0.2705) H7A(0.2044)
 H7B(0.2945) H7C(0.2611) H8A(0.4502) H8B(0.5104) H9BC(0.5782) H9BD(0.5032)
 H9AA(0.5929) H9AB(0.5392) H10A(0.4564) H10B(0.551) H10C(0.5191) H10D(0.5425)
 H10E(0.6168) H10F(0.6161) H11A(0.555) H11B(0.528) H12A(0.4446) H12B(0.4194)
 H13A(0.5517) H13B(0.4985) H13C(0.5726) H14A(0.4483) H14B(0.4838) H15A(0.5641)
 H15B(0.6012) H16A(0.5815) H16B(0.6177) H16C(0.669) H21A(0.3055) H21B(0.2972)
 H22A(0.1693) H22B(0.155) H23A(0.2726) H23B(0.1837) H23C(0.254) H24A(0.2508)
 H24B(0.1838) H25A(0.2895) H25B(0.3561) H26A(0.2699) H26B(0.328) H26C(0.3679)
 H27A(0.0706) H27B(0.1128) H28A(0.0241) H28B(0.0622) H29A(-0.0722) H29B(-
 0.0812) H29C(-0.034) H30A(0.1363) H30B(0.1527) H31A(0.2696) H31B(0.2834)
 H32A(0.2631) H32B(0.1731) H32C(0.1904) H37A(0.0138) H37B(-0.036) H38A(-0.0632)
 H38B(-0.1101) H39A(-0.1769) H39B(-0.1961) H39C(-0.1282) H40A(-0.0726) H40B(-
 0.0778) H41A(0.014) H41B(0.0006) H42A(-0.0927) H42B(-0.1461) H42C(-0.1275)
 H43A(0.0788) H43B(-0.0062) H44A(-0.0261) H44B(-0.012) H45A(0.0918)
 H45B(0.1279) H45C(0.0595) H46A(0.1973) H46B(0.282) H47A(0.2421) H47B(0.1594)
 H48A(0.2581) H48B(0.3246) H48C(0.243) H49A(-0.0071) H49B(0.0876) H49C(0.0141)
 H50A(-0.0613) H50B(-0.032) H50C(-0.0769) H51A(0.1196) H51B(0.0277)
 H52A(0.0543) H52B(0.1232) H53A(0.1204) H53B(0.2173) H53C(0.1888) H54A(0.2708)
 H54B(0.2889) H54C(0.2427) H55A(0.6464) H55B(0.6038) H55C(0.7001) H56A(0.7312)
 H56B(0.6533) H56C(0.6727) H57A(0.6053) H57B(0.6874) H58A(0.617) H58B(0.5896)
 H59A(0.4458) H59B(0.3791) H59C(0.4436) H60A(0.4871) H60B(0.4186) H60C(0.5135)
 Fixed Y: H5A(1.032) H5B(0.9921) H6A(1.0264) H6B(0.9738) H7A(1.1291)
 H7B(1.1813) H7C(1.1482) H8A(1.0039) H8B(0.9254) H9BC(0.8812) H9BD(0.9097)
 H9AA(0.9542) H9AB(0.8646) H10A(0.9859) H10B(0.9898) H10C(1.071) H10D(1.0721)
 H10E(0.9963) H10F(1.0474) H11A(0.7745) H11B(0.6557) H12A(0.817) H12B(0.6975)
 H13A(0.6608) H13B(0.7388) H13C(0.7817) H14A(0.5198) H14B(0.5452) H15A(0.6159)
 H15B(0.628) H16A(0.4347) H16B(0.4461) H16C(0.4914) H21A(0.4207) H21B(0.5326)
 H22A(0.3789) H22B(0.4932) H23A(0.3509) H23B(0.3759) H23C(0.4636) H24A(0.3214)
 H24B(0.3042) H25A(0.3313) H25B(0.3443) H26A(0.1595) H26B(0.1708) H26C(0.1791)
 H27A(0.4613) H27B(0.3579) H28A(0.4982) H28B(0.3906) H29A(0.4097) H29B(0.3754)
 H29C(0.3019) H30A(0.5226) H30B(0.6438) H31A(0.5023) H31B(0.6238) H32A(0.5994)
 H32B(0.6368) H32C(0.5167) H37A(0.6084) H37B(0.602) H38A(0.76) H38B(0.7604)
 H39A(0.6049) H39B(0.6891) H39C(0.6008) H40A(0.686) H40B(0.8048) H41A(0.6543)
 H41B(0.7719) H42A(0.6709) H42B(0.7385) H42C(0.6194) H43A(0.9798) H43B(0.9164)
 H44A(1.0584) H44B(0.9695) H45A(1.1267) H45B(1.0246) H45C(1.0931) H46A(0.9884)
 H46B(0.9232) H47A(0.8207) H47B(0.8886) H48A(0.9448) H48B(0.9646) H48C(1.0353)
 H49A(0.5905) H49B(0.5888) H49C(0.6183) H50A(0.7695) H50B(0.859) H50C(0.7579)
 H51A(0.6938) H51B(0.7233) H52A(0.8993) H52B(0.8536) H53A(1.0271) H53B(1.019)
 H53C(1.0256) H54A(0.8799) H54B(0.8475) H54C(0.7687) H55A(0.7831) H55B(0.8681)
 H55C(0.8393) H56A(0.6576) H56B(0.5833) H56C(0.6225) H57A(0.8518) H57B(0.7868)
 H58A(0.6686) H58B(0.7783) H59A(0.8449) H59B(0.7575) H59C(0.7976) H60A(0.6205)
 H60B(0.5898) H60C(0.5545)
 Fixed Z: H5A(0.42) H5B(0.417) H6A(0.4867) H6B(0.4857) H7A(0.4588) H7B(0.463)
 H7C(0.5004) H8A(0.4465) H8B(0.4738) H9BC(0.4295) H9BD(0.3955) H9AA(0.4342)
 H9AB(0.4099) H10A(0.3781) H10B(0.3728) H10C(0.4004) H10D(0.3981) H10E(0.3933)
 H10F(0.434) H11A(0.4828) H11B(0.4821) H12A(0.5145) H12B(0.5143) H13A(0.5543)
 H13B(0.5746) H13C(0.5559) H14A(0.4014) H14B(0.4456) H15A(0.386) H15B(0.4309)
 H16A(0.3913) H16B(0.4363) H16C(0.4064) H21A(0.4367) H21B(0.4546) H22A(0.4418)
 H22B(0.4563) H23A(0.4987) H23B(0.5086) H23C(0.5134) H24A(0.3966) H24B(0.3577)
 H25A(0.3227) H25B(0.362) H26A(0.3359) H26B(0.3776) H26C(0.3404) H27A(0.2863)
 H27B(0.3057) H28A(0.3432) H28B(0.3604) H29A(0.2964) H29B(0.3384) H29C(0.3137)
 H30A(0.2535) H30B(0.2592) H31A(0.2445) H31B(0.2488) H32A(0.1874) H32B(0.1928)
 H32C(0.1872) H37A(0.4147) H37B(0.3712) H38A(0.4251) H38B(0.381) H39A(0.3899)
 H39B(0.4198) H39C(0.4336) H40A(0.325) H40B(0.3125) H41A(0.2798) H41B(0.266)
 H42A(0.2236) H42B(0.2474) H42C(0.2579) H43A(0.3002) H43B(0.2959) H44A(0.327)
 H44B(0.3587) H45A(0.3488) H45B(0.3717) H45C(0.3864) H46A(0.3177) H46B(0.3298)
 H47A(0.2727) H47B(0.2605) H48A(0.2263) H48B(0.2653) H48C(0.2547) H49A(0.5358)
 H49B(0.5305) H49C(0.4951) H50A(0.4953) H50B(0.5261) H50C(0.5379) H51A(0.5829)
 H51B(0.5881) H52A(0.5798) H52B(0.6143) H53A(0.5525) H53B(0.5514) H53C(0.5916)
 H54A(0.6089) H54B(0.5682) H54C(0.5914) H55A(0.3594) H55B(0.329) H55C(0.3327)
 H56A(0.3138) H56B(0.2988) H56C(0.3422) H57A(0.2708) H57B(0.2692) H58A(0.234)
 H58B(0.2153) H59A(0.2336) H59B(0.2168) H59C(0.192) H60A(0.1869) H60B(0.2111)
 H60C(0.2254)
;