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_4087783
_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         'C68 H104 Cl2 Cu10 N4'
_chemical_formula_sum            'C68 H104 Cl2 Cu10 N4'
_chemical_formula_weight         1683.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9980(4)
_cell_length_b                   15.8415(5)
_cell_length_c                   18.0179(6)
_cell_measurement_reflns_used    4829
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      27.6600
_cell_measurement_theta_min      3.3900
_cell_volume                     3710.0(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -31.00   60.00   1.0000   28.0800
omega____ theta____ kappa____ phi______ frames
    -      -11.4829    0.0000   30.0000 91

  2 omega -101.00  -57.00   1.0000   28.0800
omega____ theta____ kappa____ phi______ frames
    -      -11.4829    0.0000   30.0000 44
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0279227000
_diffrn_orient_matrix_UB_12      -0.0246433000
_diffrn_orient_matrix_UB_13      -0.0259555000
_diffrn_orient_matrix_UB_21      0.0335792000
_diffrn_orient_matrix_UB_22      0.0135118000
_diffrn_orient_matrix_UB_23      -0.0286890000
_diffrn_orient_matrix_UB_31      0.0327424000
_diffrn_orient_matrix_UB_32      -0.0348521000
_diffrn_orient_matrix_UB_33      0.0072399000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11888
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.809
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91684
_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            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_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         1.049
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 2140 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.369(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6894
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0470P)^2^+3.7080P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.891
_reflns_Friedel_fraction_max     0.871
_reflns_number_gt                5811
_reflns_number_total             6894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00598_si_002.cif
_cod_data_source_block           2
_cod_database_code               4087783
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C104 H208 S2 Cu12'
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.759
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Others
 Fixed U13: Cu6(0) Cu5(0)
 Fixed U23: Cu6(0) Cu5(0)
 Fixed Uiso: H5(0.041) H13(0.049) H20A(0.048) H20B(0.048) H8(0.052)
 H23A(0.043) H23B(0.043) H27A(0.054) H27B(0.054) H26A(0.048) H26B(0.048)
 H24A(0.067) H24B(0.067) H16(0.06) H7(0.058) H17A(0.059) H17B(0.059)
 H19A(0.095) H19B(0.095) H19C(0.095) H21A(0.062) H21B(0.062) H6(0.056)
 H25A(0.107) H25B(0.107) H25C(0.107) H14(0.069) H15(0.083) H18A(0.089)
 H18B(0.089) H28A(0.098) H28B(0.098) H28C(0.098) H22A(0.113) H22B(0.113)
 H22C(0.113) H31A(0.103) H31B(0.103) H32A(0.131) H32B(0.131) H29A(0.164)
 H29B(0.164) H29C(0.164) H34A(0.173) H34B(0.173) H34C(0.173) H33A(0.135)
 H33B(0.135) H33C(0.135) H30A(0.174) H30B(0.174) H30C(0.174)
 Fixed X: Cu6(0) Cu5(0) H5(0.2866) H13(-0.1102) H20A(-0.0711) H20B(0.0132)
 H8(0.0599) H23A(-0.2231) H23B(-0.1343) H27A(-0.3731) H27B(-0.3098) H26A(-
 0.3374) H26B(-0.3851) H24A(-0.1004) H24B(-0.0092) H16(-0.3536) H7(0.1961)
 H17A(-0.167) H17B(-0.226) H19A(-0.3106) H19B(-0.3081) H19C(-0.3564) H21A(-
 0.109) H21B(-0.1934) H6(0.3121) H25A(-0.0352) H25B(-0.1563) H25C(-0.0777) H14(-
 0.238) H15(-0.359) H18A(-0.1457) H18B(-0.1966) H28A(-0.4569) H28B(-0.4819)
 H28C(-0.5202) H22A(-0.2279) H22B(-0.1092) H22C(-0.1726) H31A(0.3643)
 H31B(0.2949) H32A(0.4304) H32B(0.4317) H29A(0.0883) H29B(0.1662) H29C(0.1273)
 H34A(0.374) H34B(0.4665) H34C(0.4404) H33A(0.2871) H33B(0.3935) H33C(0.2882)
 H30A(0.3034) H30B(0.2985) H30C(0.1974)
 Fixed Y: Cu6(0) Cu5(0) H5(0.1387) H13(-0.0509) H20A(0.418) H20B(0.405)
 H8(0.3104) H23A(0.061) H23B(-0.0083) H27A(0.1757) H27B(0.1636) H26A(0.0131)
 H26B(0.0306) H24A(0.1702) H24B(0.1024) H16(0.1108) H7(0.2512) H17A(0.3617)
 H17B(0.2754) H19A(0.3886) H19B(0.3384) H19C(0.295) H21A(0.3292) H21B(0.3425)
 H6(0.1675) H25A(0.1477) H25B(0.1307) H25C(0.053) H14(0.0222) H15(0.1032)
 H18A(0.3278) H18B(0.2375) H28A(0.1052) H28B(0.1979) H28C(0.1167) H22A(0.4451)
 H22B(0.4708) H22C(0.4944) H31A(0.4293) H31B(0.393) H32A(0.3169) H32B(0.3096)
 H29A(0.4175) H29B(0.4812) H29C(0.3986) H34A(0.1132) H34B(0.1539) H34C(0.1885)
 H33A(0.2407) H33B(0.1903) H33C(0.1452) H30A(0.3615) H30B(0.457) H30C(0.4126)
 Fixed Z: H5(0.1878) H13(0.4431) H20A(0.1975) H20B(0.1339) H8(0.0611)
 H23A(0.0774) H23B(0.0704) H27A(0.2026) H27B(0.1272) H26A(0.1392) H26B(0.2194)
 H24A(0.07) H24B(0.0674) H16(0.3161) H7(0.0002) H17A(0.2625) H17B(0.2476)
 H19A(0.3506) H19B(0.4277) H19C(0.3555) H21A(0.0616) H21B(0.1253) H6(0.0638)
 H25A(-0.0527) H25B(-0.0473) H25C(-0.0491) H14(0.5087) H15(0.444) H18A(0.3833)
 H18B(0.3698) H28A(0.07) H28B(0.1005) H28C(0.1455) H22A(0.039) H22B(0.0322)
 H22C(0.1055) H31A(0.3413) H31B(0.4069) H32A(0.4059) H32B(0.3178) H29A(0.3017)
 H29B(0.3417) H29C(0.3843) H34A(0.3231) H34B(0.3695) H34C(0.2882) H33A(0.4693)
 H33B(0.4637) H33C(0.4403) H30A(0.2067) H30B(0.2354) H30C(0.203)
;
_olex2_submission_special_instructions 'No special instructions were received'