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_4120449
_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         'C48 H80 Cu8'
_chemical_formula_sum            'C48 H80 Cu8'
_chemical_formula_weight         1165.44
_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                 108.433(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6062(14)
_cell_length_b                   14.6470(9)
_cell_length_c                   18.6560(16)
_cell_measurement_temperature    180(2)
_cell_volume                     4823.4(7)
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30158
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.78
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.487
_exptl_absorpt_correction_T_max  0.7219
_exptl_absorpt_correction_T_min  0.7219
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'light red'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         9476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0221P)^2^+1.1643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                7720
_reflns_number_total             9476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4114243_si_002.cif
_cod_data_source_block           2b
_cod_original_cell_volume        4823.4(6)
_cod_database_code               4120449
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5A(0.033) H5B(0.033) H6A(0.059) H6B(0.059) H6C(0.059) H7A(0.041)
 H7B(0.041) H8A(0.07) H8B(0.07) H8C(0.07) H9A(0.035) H9B(0.035) H10A(0.054)
 H10B(0.054) H10C(0.054) H11A(0.029) H11B(0.029) H12A(0.051) H12B(0.051)
 H12C(0.051) H17A(0.037) H17B(0.037) H18A(0.084) H18B(0.084) H18C(0.084)
 H19A(0.048) H19B(0.048) H20A(0.083) H20B(0.083) H20C(0.083) H21A(0.043)
 H21B(0.043) H22A(0.081) H22B(0.081) H22C(0.081) H23A(0.036) H23B(0.036)
 H24A(0.083) H24B(0.083) H24C(0.083) H29A(0.041) H29B(0.041) H30A(0.091)
 H30B(0.091) H30C(0.091) H31A(0.05) H31B(0.05) H32A(0.078) H32B(0.078)
 H32C(0.078) H33A(0.055) H33B(0.055) H34A(0.077) H34B(0.077) H34C(0.077)
 H35A(0.035) H35B(0.035) H36A(0.072) H36B(0.072) H36C(0.072) H41A(0.04)
 H41B(0.04) H42A(0.062) H42B(0.062) H42C(0.062) H43A(0.044) H43B(0.044)
 H44A(0.062) H44B(0.062) H44C(0.062) H45A(0.036) H45B(0.036) H46A(0.048)
 H46B(0.048) H46C(0.048) H47A(0.03) H47B(0.03) H48A(0.05) H48B(0.05) H48C(0.05)
 Fixed X: H5A(0.3593) H5B(0.4196) H6A(0.2917) H6B(0.3454) H6C(0.288)
 H7A(0.4972) H7B(0.5113) H8A(0.6263) H8B(0.6152) H8C(0.6293) H9A(0.5134)
 H9B(0.5344) H10A(0.4086) H10B(0.4126) H10C(0.3841) H11A(0.5494) H11B(0.6013)
 H12A(0.6438) H12B(0.695) H12C(0.6805) H17A(0.4798) H17B(0.5643) H18A(0.5118)
 H18B(0.5007) H18C(0.5842) H19A(0.6697) H19B(0.7173) H20A(0.7922) H20B(0.7896)
 H20C(0.7386) H21A(0.7617) H21B(0.7368) H22A(0.6587) H22B(0.626) H22C(0.7025)
 H23A(0.7073) H23B(0.7382) H24A(0.8284) H24B(0.8383) H24C(0.7958) H29A(0.2974)
 H29B(0.337) H30A(0.3047) H30B(0.3466) H30C(0.3951) H31A(0.3081) H31B(0.3663)
 H32A(0.2944) H32B(0.3337) H32C(0.3835) H33A(0.5671) H33B(0.4801) H34A(0.4606)
 H34B(0.5355) H34C(0.5422) H35A(0.6374) H35B(0.6436) H36A(0.5612) H36B(0.5626)
 H36C(0.6386) H41A(0.2467) H41B(0.202) H42A(0.1821) H42B(0.271) H42C(0.2218)
 H43A(0.2302) H43B(0.2387) H44A(0.333) H44B(0.252) H44C(0.3169) H45A(0.3138)
 H45B(0.3996) H46A(0.3309) H46B(0.4163) H46C(0.3473) H47A(0.5075) H47B(0.5705)
 H48A(0.521) H48B(0.4623) H48C(0.5513)
 Fixed Y: H5A(0.3664) H5B(0.435) H6A(0.4921) H6B(0.5618) H6C(0.4978)
 H7A(0.526) H7B(0.6107) H8A(0.5649) H8B(0.464) H8C(0.5476) H9A(0.6363)
 H9B(0.6584) H10A(0.6513) H10B(0.7158) H10C(0.6126) H11A(0.5488) H11B(0.4601)
 H12A(0.6186) H12B(0.5286) H12C(0.5888) H17A(0.303) H17B(0.3291) H18A(0.222)
 H18B(0.151) H18C(0.1791) H19A(0.2916) H19B(0.2043) H20A(0.3393) H20B(0.2934)
 H20C(0.3811) H21A(0.1329) H21B(0.0973) H22A(0.0614) H22B(0.033) H22C(-0.0124)
 H23A(0.2495) H23B(0.1652) H24A(0.2606) H24B(0.2679) H24C(0.3473) H29A(0.0805)
 H29B(0.1451) H30A(0.0089) H30B(-0.0501) H30C(0.0111) H31A(-0.0015) H31B(-
 0.0805) H32A(-0.0268) H32B(0.071) H32C(-0.0159) H33A(-0.0893) H33B(-0.1165)
 H34A(-0.121) H34B(-0.1792) H34C(-0.0778) H35A(0.0051) H35B(0.1026) H36A(-
 0.0495) H36B(0.0488) H36C(-0.0105) H41A(0.1792) H41B(0.2656) H42A(0.2493)
 H42B(0.262) H42C(0.345) H43A(0.3042) H43B(0.2048) H44A(0.171) H44B(0.192)
 H44C(0.2682) H45A(0.4111) H45B(0.4327) H46A(0.4936) H46B(0.5159) H46C(0.5577)
 H47A(0.3972) H47B(0.3287) H48A(0.2106) H48B(0.2826) H48C(0.2953)
 Fixed Z: H5A(0.544) H5B(0.528) H6A(0.4781) H6B(0.5373) H6C(0.5625)
 H7A(0.5649) H7B(0.6217) H8A(0.6071) H8B(0.6347) H8C(0.6927) H9A(0.8129)
 H9B(0.738) H10A(0.6644) H10B(0.7348) H10C(0.7335) H11A(0.8982) H11B(0.9245)
 H12A(0.8571) H12B(0.8778) H12C(0.9435) H17A(0.5252) H17B(0.5285) H18A(0.4314)
 H18B(0.4923) H18C(0.4934) H19A(0.5677) H19B(0.6071) H20A(0.6311) H20B(0.7081)
 H20C(0.6752) H21A(0.7206) H21B(0.7903) H22A(0.6355) H22B(0.702) H22C(0.6971)
 H23A(0.9152) H23B(0.8786) H24A(0.8515) H24B(0.9397) H24C(0.8833) H29A(0.6134)
 H29B(0.5674) H30A(0.4998) H30B(0.5734) H30C(0.5344) H31A(0.6965) H31B(0.7367)
 H32A(0.8139) H32B(0.8175) H32C(0.855) H33A(0.8244) H33B(0.8075) H34A(0.6796)
 H34B(0.7191) H34C(0.69) H35A(0.8777) H35B(0.9179) H36A(0.9475) H36B(0.9854)
 H36C(1.0045) H41A(0.6921) H41B(0.7088) H42A(0.5776) H42B(0.5921) H42C(0.6073)
 H43A(0.8503) H43B(0.819) H44A(0.9363) H44B(0.9457) H44C(0.9672) H45A(0.9136)
 H45B(0.9627) H46A(0.8109) H46B(0.8606) H46C(0.8838) H47A(0.9894) H47B(0.9785)
 H48A(1.0389) H48B(1.0533) H48C(1.0945)
;