Well-Defined Butadienyl Organocopper(I) Aggregates from Zirconacyclopentadienes and CuCl: Synthesis and Structural Characterization
Liu, Liang; Geng, Weizhi; Yang, Qi; Zhang, Wen-Xiong; Xi, Zhenfeng; Organometallics 34 (2015) 4198–; doi:10.1021/acs.organomet.5b00598

data_4087784
_publ_section_title
;
 Well-Defined Butadienyl Organocopper(I) Aggregates from
 Zirconacyclopentadienes and CuCl: Synthesis and Structural
 Characterization
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4198
_journal_paper_doi               10.1021/acs.organomet.5b00598
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C92 H124 Cu12 S2'
_chemical_formula_sum            'C92 H124 Cu12 S2'
_chemical_formula_weight         2056.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                96.035(3)
_cell_angle_beta                 113.105(4)
_cell_angle_gamma                110.051(4)
_cell_formula_units_Z            1
_cell_length_a                   12.6667(5)
_cell_length_b                   13.5072(6)
_cell_length_c                   15.0381(6)
_cell_measurement_reflns_used    6811
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      28.0540
_cell_measurement_theta_min      3.3260
_cell_volume                     2135.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      180.01(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   35.00   60.00   1.0000    4.5100
omega____ theta____ kappa____ phi______ frames
    -       10.8579 -178.0000  120.0000 25

  2 omega   -3.00   24.00   1.0000    4.5100
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -99.0000  -90.0000 27

  3 omega  -14.00   12.00   1.0000    4.5100
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -99.0000  150.0000 26

  4 omega   -3.00   22.00   1.0000    4.5100
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -99.0000 -120.0000 25

  5 omega  -37.00   58.00   1.0000    4.5100
omega____ theta____ kappa____ phi______ frames
    -      -11.6392   38.0000  -90.0000 95

  6 omega  -15.00   29.00   1.0000    4.5100
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -99.0000  -30.0000 44

  7 omega  -79.00  -38.00   1.0000    4.5100
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -38.0000  -30.0000 41

  8 omega  -15.00   11.00   1.0000    4.5100
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -38.0000  -30.0000 26

  9 omega  -41.00   47.00   1.0000    4.5100
omega____ theta____ kappa____ phi______ frames
    -      -11.6392   57.0000  150.0000 88
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0224086000
_diffrn_orient_matrix_UB_12      0.0041974000
_diffrn_orient_matrix_UB_13      0.0521195000
_diffrn_orient_matrix_UB_21      -0.0267448000
_diffrn_orient_matrix_UB_22      0.0373610000
_diffrn_orient_matrix_UB_23      0.0047361000
_diffrn_orient_matrix_UB_31      -0.0572942000
_diffrn_orient_matrix_UB_32      -0.0444070000
_diffrn_orient_matrix_UB_33      -0.0104892000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20006
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.961
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.013
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light black'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.476
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8406
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+3.4270P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6350
_reflns_number_total             8406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00598_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        2135.82(17)
_cod_database_code               4087784
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C52 H'
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.753
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_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. Rigid bond restraints
 C38, C38, C37, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C38, C38, C37, C37
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C7, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C38) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C38) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C34(H34A,H34B), C40(H40A,H40B), C26(H26A,H26B), C32(H32A,
 H32B), C25(H25A,H25B), C29(H29A,H29B), C28(H28A,H28B), C35(H35A,H35B),
 C41(H41A,H41B), C37(H37A,H37B), C43(H43A,H43B), C46(H46A,H46B), C44(H44A,H44B),
  C45(H45A,H45B), C38(H38A,H38B)
4.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C13(H13), C16(H16), C14(H14), C15(H15), C24(H24), C22(H22), C5(H5),
 C23(H23), C6(H6), C8(H8), C7(H7)
4.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C42(H42A,H42B,H42C), C33(H33A,H33B,H33C), C36(H36A,H36B,
 H36C), C39(H39A,H39B,H39C), C30(H30A,H30B,H30C)
;
_olex2_submission_special_instructions 'No special instructions were received'