Aromatic Dicupra[10]annulenes.
Wei, Junnian; Zhang, Yongliang; Chi, Yue; Liu, Liang; Zhang, Wen-Xiong; Xi, Zhenfeng; Journal of the American Chemical Society 138 (2016) 60–63; doi:10.1021/jacs.5b11317

data_4129880
_publ_section_title
;
 Aromatic Dicupra[10]annulenes.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              60
_journal_page_last               63
_journal_paper_doi               10.1021/jacs.5b11317
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C52 H72 Cu2 Li2 O2 Si4'
_chemical_formula_sum            'C52 H72 Cu2 Li2 O2 Si4'
_chemical_formula_weight         982.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.4610(8)
_cell_length_b                   10.7746(3)
_cell_length_c                   20.9554(7)
_cell_measurement_reflns_used    8413
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      26.0500
_cell_measurement_theta_min      3.2610
_cell_volume                     5523.0(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -35.00   54.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7173   57.0000  120.0000 89

  2 omega  -67.00   18.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7173  -57.0000 -180.0000 85

  3 omega  -86.00   18.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7173  -57.0000  -30.0000 104
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0219745000
_diffrn_orient_matrix_UB_12      -0.0063361000
_diffrn_orient_matrix_UB_13      0.0218179000
_diffrn_orient_matrix_UB_21      0.0189150000
_diffrn_orient_matrix_UB_22      -0.0102754000
_diffrn_orient_matrix_UB_23      0.0251235000
_diffrn_orient_matrix_UB_31      0.0008553000
_diffrn_orient_matrix_UB_32      0.0647208000
_diffrn_orient_matrix_UB_33      0.0061251000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35206
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.13
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67795
_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 red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.522(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         10811
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+4.1189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1432
_reflns_number_gt                7756
_reflns_number_total             10811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b11317_si_002.cif
_cod_data_source_block           14may23g
_cod_database_code               4129880
_chemical_oxdiff_formula         'C20 H20 N4 O2 Si2 Cu2 Li2'
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H10(0.058) H11(0.073) H12(0.069) H13(0.066) H14(0.055) H16(0.071)
 H17(0.106) H18(0.122) H19(0.102) H20(0.072) H22(0.062) H23(0.081) H24(0.08)
 H25(0.077) H26(0.063) H27(0.055) H28(0.065) H29(0.07) H30(0.069) H31(0.057)
 H33A(0.182) H33B(0.182) H33C(0.182) H34A(0.125) H34B(0.125) H34C(0.125)
 H35A(0.161) H35B(0.161) H35C(0.161) H36A(0.091) H36B(0.091) H36C(0.091)
 H37A(0.105) H37B(0.105) H37C(0.105) H38A(0.107) H38B(0.107) H38C(0.107)
 H39A(0.148) H39B(0.148) H39C(0.148) H40A(0.122) H40B(0.122) H40C(0.122)
 H41A(0.104) H41B(0.104) H41C(0.104) H42A(0.149) H42B(0.149) H42C(0.149)
 H43A(0.134) H43B(0.134) H43C(0.134) H44A(0.144) H44B(0.144) H44C(0.144)
 H45A(0.088) H45B(0.088) H46A(0.125) H46B(0.125) H46C(0.125) H46D(0.125)
 H47A(0.085) H47B(0.085) H47C(0.139) H47D(0.139) H48A(0.146) H48B(0.146)
 H48C(0.146) H48D(0.146) H49A(0.067) H49B(0.067) H50A(0.086) H50B(0.086)
 H51A(0.079) H51B(0.079) H52A(0.089) H52B(0.089)
 Fixed X: H10(0.5863) H11(0.6747) H12(0.6912) H13(0.6191) H14(0.5307)
 H16(0.4679) H17(0.5115) H18(0.5596) H19(0.5651) H20(0.5212) H22(0.2867)
 H23(0.2395) H24(0.1902) H25(0.1847) H26(0.2285) H27(0.2238) H28(0.135)
 H29(0.062) H30(0.0774) H31(0.1653) H33A(0.5238) H33B(0.557) H33C(0.5784)
 H34A(0.4287) H34B(0.4709) H34C(0.4354) H35A(0.5848) H35B(0.5627) H35C(0.533)
 H36A(0.3029) H36B(0.2725) H36C(0.2728) H37A(0.3178) H37B(0.3089) H37C(0.3658)
 H38A(0.4149) H38B(0.3589) H38C(0.403) H39A(0.3225) H39B(0.2815) H39C(0.3183)
 H40A(0.2197) H40B(0.1871) H40C(0.1686) H41A(0.18) H41B(0.1829) H41C(0.2286)
 H42A(0.4516) H42B(0.4759) H42C(0.4819) H43A(0.3262) H43B(0.3848) H43C(0.3563)
 H44A(0.4194) H44B(0.4379) H44C(0.3768) H45A(0.4892) H45B(0.434) H46A(0.4026)
 H46B(0.465) H46C(0.4254) H46D(0.4663) H47A(0.4606) H47B(0.4002) H47C(0.3914)
 H47D(0.3588) H48A(0.3656) H48B(0.4156) H48C(0.372) H48D(0.4312) H49A(0.2615)
 H49B(0.3086) H50A(0.3589) H50B(0.2996) H51A(0.3631) H51B(0.3013) H52A(0.3908)
 H52B(0.3392)
 Fixed Y: H10(0.8808) H11(0.9147) H12(1.0366) H13(1.1067) H14(1.0586)
 H16(0.8315) H17(0.682) H18(0.5262) H19(0.5268) H20(0.6749) H22(0.7918)
 H23(0.6289) H24(0.4933) H25(0.5161) H26(0.6821) H27(1.0278) H28(1.0617)
 H29(1.0079) H30(0.9216) H31(0.8945) H33A(1.0308) H33B(1.1552) H33C(1.043)
 H34A(1.2679) H34B(1.3235) H34C(1.2083) H35A(1.1968) H35B(1.3157) H35C(1.2656)
 H36A(0.6855) H36B(0.6456) H36C(0.7853) H37A(0.8676) H37B(0.7288) H37C(0.7922)
 H38A(0.5762) H38B(0.5192) H38C(0.555) H39A(1.2747) H39B(1.3185) H39C(1.2014)
 H40A(1.0404) H40B(1.1655) H40C(1.0512) H41A(1.1989) H41B(1.3073) H41C(1.2936)
 H42A(0.7033) H42B(0.6235) H42C(0.7684) H43A(0.5508) H43B(0.4922) H43C(0.542)
 H44A(0.8113) H44B(0.672) H44C(0.7069) H45A(1.2788) H45B(1.3362) H46A(1.3706)
 H46B(1.369) H46C(1.4073) H46D(1.308) H47A(1.1767) H47B(1.2201) H47C(1.2409)
 H47D(1.2832) H48A(1.1258) H48B(1.0363) H48C(1.0733) H48D(1.0732) H49A(1.2619)
 H49B(1.3244) H50A(1.3676) H50B(1.3812) H51A(1.227) H51B(1.1871) H52A(1.119)
 H52B(1.038)
 Fixed Z: H10(0.0805) H11(0.0466) H12(-0.0421) H13(-0.1017) H14(-0.0737) H16(-
 0.132) H17(-0.1897) H18(-0.1391) H19(-0.0297) H20(0.0286) H22(0.2946)
 H23(0.3421) H24(0.2815) H25(0.1724) H26(0.1252) H27(0.2481) H28(0.2835)
 H29(0.2192) H30(0.1213) H31(0.085) H33A(0.2189) H33B(0.2208) H33C(0.1802)
 H34A(0.1236) H34B(0.1721) H34C(0.1914) H35A(0.0626) H35B(0.0972) H35C(0.0361)
 H36A(0.0448) H36B(-0.0178) H36C(0.0032) H37A(-0.1229) H37B(-0.1428) H37C(-
 0.1538) H38A(-0.0824) H38B(-0.0607) H38C(-0.0097) H39A(0.0447) H39B(-0.0082)
 H39C(-0.0197) H40A(-0.0473) H40B(-0.0436) H40C(-0.0025) H41A(0.1273)
 H41B(0.0776) H41C(0.1295) H42A(0.1117) H42B(0.1675) H42C(0.1685) H43A(0.2078)
 H43B(0.2038) H43C(0.1419) H44A(0.2949) H44B(0.2963) H44C(0.3105) H45A(-0.0771)
 H45B(-0.0519) H46A(-0.1496) H46B(-0.168) H46C(-0.1506) H46D(-0.1784) H47A(-
 0.2057) H47B(-0.2211) H47C(-0.2137) H47D(-0.1524) H48A(-0.1339) H48B(-0.1447)
 H48C(-0.1297) H48D(-0.1603) H49A(0.2562) H49B(0.216) H50A(0.3038) H50B(0.333)
 H51A(0.3841) H51B(0.3748) H52A(0.3017) H52B(0.3185)
;