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_4120452
_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         'C44 H80 Cu3 I2 Li O3'
_chemical_formula_sum            'C44 H80 Cu3 I2 Li O3'
_chemical_formula_weight         1108.44
_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     iterative
_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                95.008(3)
_cell_angle_beta                 99.948(3)
_cell_angle_gamma                98.618(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1034(3)
_cell_length_b                   12.6088(5)
_cell_length_c                   22.6274(9)
_cell_measurement_temperature    100(2)
_cell_volume                     2512.17(17)
_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
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23828
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.520
_exptl_absorpt_correction_T_max  0.7867
_exptl_absorpt_correction_T_min  0.6326
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.714
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         9875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0737P)^2^+2.4919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1451
_reflns_number_gt                7820
_reflns_number_total             9875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4114243_si_002.cif
_cod_data_source_block           5
_cod_original_cell_volume        2512.17(16)
_cod_database_code               4120452
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H9A(0.042) H9B(0.042) H10A(0.071) H10B(0.071) H11A(0.078)
 H11B(0.078) H11C(0.078) H12A(0.033) H12B(0.033) H13A(0.047) H13B(0.047)
 H14A(0.067) H14B(0.067) H14C(0.067) H15A(0.04) H15B(0.04) H16A(0.048)
 H16B(0.048) H17A(0.083) H17B(0.083) H17C(0.083) H18A(0.033) H18B(0.033)
 H19A(0.041) H19B(0.041) H20A(0.077) H20B(0.077) H20C(0.077) H21A(0.029)
 H21B(0.029) H22A(0.036) H22B(0.036) H23A(0.063) H23B(0.063) H23C(0.063)
 H24A(0.031) H24B(0.031) H25A(0.043) H25B(0.043) H26A(0.07) H26B(0.07)
 H26C(0.07) H27A(0.031) H27B(0.031) H28A(0.041) H28B(0.041) H29A(0.064)
 H29B(0.064) H29C(0.064) H30A(0.04) H30B(0.04) H31A(0.059) H31B(0.059)
 H32A(0.095) H32B(0.095) H32C(0.095) H33A(0.088) H33B(0.088) H34A(0.102)
 H34B(0.102) H35A(0.087) H35B(0.087) H36A(0.081) H36B(0.081) H37A(0.146)
 H37B(0.146) H38A(0.096) H38B(0.096) H39A(0.146) H39B(0.146) H40A(0.146)
 H40B(0.146) H41A(0.09) H41B(0.09) H42A(0.119) H42B(0.119) H43A(0.137)
 H43B(0.137) H44A(0.146) H44B(0.146)
 Fixed X: H9A(0.4475) H9B(0.486) H10A(0.4899) H10B(0.5104) H11A(0.7194)
 H11B(0.7425) H11C(0.7429) H12A(0.3056) H12B(0.1299) H13A(0.2726) H13B(0.093)
 H14A(0.1267) H14B(0.1926) H14C(0.3051) H15A(-0.1786) H15B(-0.0648) H16A(-
 0.1384) H16B(-0.2432) H17A(-0.3009) H17B(-0.3825) H17C(-0.4123) H18A(-0.1625)
 H18B(-0.2376) H19A(-0.2391) H19B(-0.1622) H20A(-0.458) H20B(-0.4254) H20C(-
 0.381) H21A(0.2408) H21B(0.2628) H22A(0.0003) H22B(0.0375) H23A(0.2565)
 H23B(0.1044) H23C(0.2091) H24A(0.1778) H24B(0.2121) H25A(0.401) H25B(0.4336)
 H26A(0.4613) H26B(0.5857) H26C(0.4426) H27A(-0.0849) H27B(-0.1234)
 H28A(0.0704) H28B(0.1005) H29A(-0.1434) H29B(-0.054) H29C(-0.1782)
 H30A(0.1137) H30B(-0.0413) H31A(0.2062) H31B(0.0534) H32A(0.0519) H32B(0.0682)
 H32C(-0.0828) H33A(0.3445) H33B(0.3623) H34A(0.3421) H34B(0.3578) H35A(0.5792)
 H35B(0.5881) H36A(0.7492) H36B(0.6589) H37A(0.9868) H37B(0.9544) H38A(1.1858)
 H38B(1.1663) H39A(1.1031) H39B(1.1289) H40A(0.8679) H40B(0.8469) H41A(0.4512)
 H41B(0.6237) H42A(0.3659) H42B(0.5326) H43A(0.5987) H43B(0.4182) H44A(0.5689)
 H44B(0.3971)
 Fixed Y: H9A(0.6448) H9B(0.7635) H10A(0.7113) H10B(0.8326) H11A(0.6941)
 H11B(0.7748) H11C(0.8218) H12A(0.6303) H12B(0.6069) H13A(0.4881) H13B(0.4694)
 H14A(0.4158) H14B(0.3386) H14C(0.43) H15A(0.6523) H15B(0.5679) H16A(0.5341)
 H16B(0.6252) H17A(0.4358) H17B(0.4446) H17C(0.5216) H18A(0.906) H18B(0.7832)
 H19A(0.8172) H19B(0.9401) H20A(0.8466) H20B(0.9311) H20C(0.9687) H21A(0.8103)
 H21B(0.9314) H22A(0.7749) H22B(0.8936) H23A(0.8449) H23B(0.7708) H23C(0.7249)
 H24A(1.1634) H24B(1.0789) H25A(1.1454) H25B(1.0547) H26A(1.1877) H26B(1.2165)
 H26C(1.2772) H27A(1.1117) H27B(1.0848) H28A(1.2314) H28B(1.26) H29A(1.3034)
 H29B(1.374) H29C(1.2709) H30A(1.1012) H30B(1.0246) H31A(0.9537) H31B(0.8755)
 H32A(1.0483) H32B(0.9294) H32C(0.9494) H33A(1.4148) H33B(1.2966) H34A(1.3576)
 H34B(1.4801) H35A(1.4966) H35B(1.3702) H36A(1.4378) H36B(1.5354) H37A(1.3513)
 H37B(1.225) H38A(1.2676) H38B(1.3899) H39A(1.3481) H39B(1.2266) H40A(1.1676)
 H40B(1.2617) H41A(1.3806) H41B(1.3868) H42A(1.2877) H42B(1.3221) H43A(1.1651)
 H43B(1.1231) H44A(1.1114) H44B(1.1308)
 Fixed Z: H9A(0.2019) H9B(0.183) H10A(0.3022) H10B(0.286) H11A(0.2649)
 H11B(0.3256) H11C(0.2622) H12A(0.0983) H12B(0.0681) H13A(0.1574) H13B(0.1349)
 H14A(0.0356) H14B(0.0823) H14C(0.06) H15A(0.176) H15B(0.1732) H16A(0.068)
 H16B(0.0678) H17A(0.1263) H17B(0.0588) H17C(0.114) H18A(0.163) H18B(0.1401)
 H19A(0.0385) H19B(0.0612) H20A(0.0768) H20B(0.03) H20C(0.101) H21A(0.0837)
 H21B(0.0672) H22A(0.0148) H22B(-0.0047) H23A(-0.0382) H23B(-0.075) H23C(-
 0.0222) H24A(0.1309) H24B(0.0804) H25A(0.1965) H25B(0.1488) H26A(0.0803)
 H26B(0.1412) H26C(0.1319) H27A(0.1566) H27B(0.2205) H28A(0.2692) H28B(0.2044)
 H29A(0.1806) H29B(0.242) H29C(0.2441) H30A(0.3344) H30B(0.3031) H31A(0.3744)
 H31B(0.342) H32A(0.4311) H32B(0.448) H32C(0.4057) H33A(0.3629) H33B(0.3351)
 H34A(0.2465) H34B(0.2767) H35A(0.2482) H35B(0.2498) H36A(0.3357) H36B(0.3479)
 H37A(0.3728) H37B(0.3813) H38A(0.4361) H38B(0.4544) H39A(0.5339) H39B(0.5167)
 H40A(0.4722) H40B(0.522) H41A(0.5003) H41B(0.5335) H42A(0.5663) H42B(0.607)
 H43A(0.5823) H43B(0.569) H44A(0.4872) H44B(0.4738)
;