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_4087786
_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         'C48 H92 Cl4 Cu10 N4'
_chemical_formula_sum            'C48 H92 Cl4 Cu10 N4'
_chemical_formula_weight         1502.45
_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                87.633(2)
_cell_angle_beta                 83.322(3)
_cell_angle_gamma                62.031(4)
_cell_formula_units_Z            2
_cell_length_a                   11.8027(5)
_cell_length_b                   12.3566(4)
_cell_length_c                   24.9990(5)
_cell_measurement_reflns_used    11396
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      28.0810
_cell_measurement_theta_min      3.3430
_cell_volume                     3197.8(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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -17.00   57.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017   57.0000    0.0000 74

  2 omega   45.00   97.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017 -178.0000  120.0000 52

  3 omega  -20.00    6.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  -38.0000 -180.0000 26

  4 omega  -86.00   15.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4829  -43.0000   97.0000 101

  5 omega  -19.00   14.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4829  -99.0000  120.0000 33

  6 omega  -58.00   52.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4829   19.0000  -60.0000 110
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0483872000
_diffrn_orient_matrix_UB_12      0.0512028000
_diffrn_orient_matrix_UB_13      0.0153059000
_diffrn_orient_matrix_UB_21      -0.0446691000
_diffrn_orient_matrix_UB_22      -0.0226848000
_diffrn_orient_matrix_UB_23      -0.0016924000
_diffrn_orient_matrix_UB_31      0.0187073000
_diffrn_orient_matrix_UB_32      -0.0329964000
_diffrn_orient_matrix_UB_33      0.0240649000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            30460
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         3.009
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.452
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92070
_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            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       block
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         1.847
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         12575
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0570P)^2^+3.0050P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9543
_reflns_number_total             12575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00598_si_002.cif
_cod_data_source_block           6
_cod_database_code               4087786
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C50 H100 Cu10 Cl4 N4'
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.724
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C27
 1.54 with sigma of 0.02
3. Rigid bond restraints
 C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C30, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27, C28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C30) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C28) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C28) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C28) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C19(H19A,H19B), C33(H33A,H33B), C23(H23A,H23B), C35(H35A,
 H35B), C21(H21A,H21B), C31(H31A,H31B), C17(H17A,H17B), C13(H13A,H13B),
 C44(H44A,H44B), C29(H29A,H29B), C38(H38A,H38B), C25(H25A,H25B), C43(H43A,H43B),
  C37(H37A,H37B), C27(H27A,H27B)
5.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C20(H20A,H20B,
 H20C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C45(H45A,H45B,H45C), C41(H41A,
 H41B,H41C), C32(H32A,H32B,H32C), C47(H47A,H47B,H47C), C36(H36A,H36B,H36C),
 C39(H39A,H39B,H39C), C14(H14A,H14B,H14C), C46(H46A,H46B,H46C), C40(H40A,H40B,
 H40C), C26(H26A,H26B,H26C), C42(H42A,H42B,H42C), C48(H48A,H48B,H48C), C30(H30A,
 H30B,H30C), C28(H28A,H28B,H28C)
;
_olex2_submission_special_instructions 'No special instructions were received'