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_4087785
_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         'C60 H116 Cl4 Cu10 N4'
_chemical_formula_sum            'C60 H116 Cl4 Cu10 N4'
_chemical_formula_weight         1670.76
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 100.552(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.307(3)
_cell_length_b                   13.054(2)
_cell_length_c                   35.207(6)
_cell_measurement_temperature    173.15
_cell_volume                     7368(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'RIGAKU CCD SATURN724'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            55143
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         1.177
_exptl_absorpt_coefficient_mu    3.005
_exptl_absorpt_correction_T_max  0.618
_exptl_absorpt_correction_T_min  0.554
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'orangish yellow'
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       block
_exptl_crystal_F_000             3448
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.571
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         16813
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0836
_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^)+(0.0885P)^2^+22.8158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2124
_refine_ls_wR_factor_ref         0.2263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14169
_reflns_number_total             16813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00598_si_002.cif
_cod_data_source_block           5
_cod_database_code               4087785
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.645
_shelx_estimated_absorpt_t_min   0.585
_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
 C44-C45 = C20-C21
 1.54 with sigma of 0.01
 C51-C52
 1.5 with sigma of 0.02
 N1-C52 \\sim N2-C51 \\sim N2-C51
 with sigma of 0.02
3. Rigid bond restraints
 N2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21, C52, C54
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21, C52, C54
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C52
 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(C52) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C39) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C21) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C21) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C21) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
5.a Riding coordinates:
 C53(H53A,H53B,H53C)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,
 H19B), C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B),
 C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B), C32(H32A,H32B),
  C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B), C40(H40A,
 H40B), C41(H41A,H41B), C43(H43A,H43B), C44(H44A,H44B), C46(H46A,H46B),
 C47(H47A,H47B), C57(H57A,H57B), C58(H58A,H58B), C51(H51A,H51B), C52(H52A,H52B)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C24(H24A,H24B,
 H24C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C36(H36A,
 H36B,H36C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C),
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C54(H54A,H54B,
 H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C)
;
_olex2_submission_special_instructions 'No special instructions were received'