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_4129879
_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_formula_moiety         'C44 H84 Cu2 Li4 O4 Si4'
_chemical_formula_sum            'C44 H84 Cu2 Li4 O4 Si4'
_chemical_formula_weight         944.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 93.795(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3581(4)
_cell_length_b                   22.2386(8)
_cell_length_c                   19.3513(7)
_cell_measurement_reflns_used    7848
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      28.4430
_cell_measurement_theta_min      2.9360
_cell_volume                     5306.6(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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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  -19.00   10.00   1.0000   16.3200
omega____ theta____ kappa____ phi______ frames
    -       10.5454  -99.0000    0.0000 29

  2 omega  -10.00   82.00   1.0000   16.3200
omega____ theta____ kappa____ phi______ frames
    -       10.5454   19.0000  -60.0000 92

  3 omega   -3.00   85.00   1.0000   16.3200
omega____ theta____ kappa____ phi______ frames
    -       10.5454   38.0000 -180.0000 88

  4 omega  -10.00   15.00   1.0000   16.3200
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -99.0000  -30.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0557826000
_diffrn_orient_matrix_UB_12      -0.0077858000
_diffrn_orient_matrix_UB_13      0.0013503000
_diffrn_orient_matrix_UB_21      0.0047195000
_diffrn_orient_matrix_UB_22      0.0135306000
_diffrn_orient_matrix_UB_23      -0.0328690000
_diffrn_orient_matrix_UB_31      0.0132958000
_diffrn_orient_matrix_UB_32      0.0277835000
_diffrn_orient_matrix_UB_33      0.0163848000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28285
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.91
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10619
_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    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         10444
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+3.0383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1569
_reflns_number_gt                7238
_reflns_number_total             10444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b11317_si_002.cif
_cod_data_source_block           exp_5507
_cod_database_code               4129879
_chemical_oxdiff_formula         'C20 H30 Si4 Cu2 O4 Li4'
_reflns_odcompleteness_completeness 99.78
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C42-C43
 1.54 with sigma of 0.02
 C42-C41
 1.54 with sigma of 0.02
 C43-C44
 1.54 with sigma of 0.02
3. Rigid bond restraints
 O1, C29, C30, C31, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C41, C42, C43, C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C29 \\sim C30 \\sim C31 \\sim C32: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C35) \\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C39A)
\\sim Ueq, Uanis(C40A) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Others
 Sof(H33C)=Sof(H33D)=Sof(H36C)=Sof(H36D)=Sof(H38C)=Sof(H38D)=Sof(C34)=
 Sof(H34C)=Sof(H34D)=Sof(C35)=Sof(H35C)=Sof(H35D)=Sof(C39A)=Sof(H39C)=Sof(H39D)=
 Sof(C40A)=Sof(H40C)=Sof(H40D)=1-FVAR(1)
 Sof(H33A)=Sof(H33B)=Sof(H36A)=Sof(H36B)=Sof(H38A)=Sof(H38B)=Sof(C34A)=
 Sof(H34A)=Sof(H34B)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C29(H29A,H29B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C33(H33C,H33D), C36(H36A,
 H36B), C36(H36C,H36D), C37(H37A,H37B), C38(H38A,H38B), C38(H38C,H38D),
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C34A(H34A,
 H34B), C35A(H35A,H35B), C39(H39A,H39B), C40(H40A,H40B), C34(H34C,H34D),
 C35(H35C,H35D), C39A(H39C,H39D), C40A(H40C,H40D)
6.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
 C28(H28A,H28B,H28C)
;
_olex2_submission_special_instructions 'No special instructions were received'