The crystal structure of dichlorido-μ2-dichlorido-(η2-1,4-bis(4-vinylbenzyl)-1,4-diazabicyclo[2.2.2]octane-1,4-diium)dicopper(I), C24H30N2Cu2Cl4
Wang, Guo-Xi; Xing, Zheng; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 997–999; doi:10.1515/ncrs-2019-0212

data_8105917
_publ_section_title
;
 The crystal structure of
 dichlorido-\m2-dichlorido-(\h2-1,4-bis(4-vinylbenzyl)-1,4-diazabicyclo[2.2.2]octane-1,4-diium)dicopper(I),
 C24H30N2Cu2Cl4
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              997
_journal_page_last               999
_journal_paper_doi               10.1515/ncrs-2019-0212
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C24 H30 Cl4 Cu2 N2'
_chemical_formula_sum            'C24 H30 Cl4 Cu2 N2'
_chemical_formula_weight         615.38
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                89.153(7)
_cell_angle_beta                 85.294(7)
_cell_angle_gamma                84.604(6)
_cell_formula_units_Z            2
_cell_length_a                   7.204(4)
_cell_length_b                   8.593(5)
_cell_length_c                   21.112(12)
_cell_measurement_reflns_used    4131
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.328
_cell_measurement_theta_min      2.563
_cell_volume                     1296.7(13)
_computing_cell_refinement       'Bruker SMART [1]'
_computing_data_collection       'Bruker SMART [1]'
_computing_data_reduction        'Bruker SMART [1]'
_computing_molecular_graphics    'Olex2 -2009)[4]'
_computing_publication_material  Olex2-2009)[4]
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)[3]'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)[2]'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20772
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.849
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.068
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.420
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4567
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+1.2190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3021
_reflns_number_total             4567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0212_suppl.cif
_cod_data_source_block           11
_cod_original_cell_volume        1296.7(12)
_cod_database_code               8105917
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.707
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C23A-C20A
 1.48 with sigma of 0.02
 C17A-C16
 1.5 with sigma of 0.02
 C24-C23
 1.33 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C19A)
\\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C22A) \\sim Ueq,
Uanis(C23A) \\sim Ueq, Uanis(C24A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cu2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23A) = Uanis(C23)
Uanis(C24) = Uanis(C24A)
4. Others
 Sof(H16C)=Sof(H16D)=Sof(C17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=
 Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=
 Sof(C24A)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=
 Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C2(H2)
5.b 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), C16(H16C,H16D)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C18(H18), C19(H19), C21(H21), C22(H22),
 C23(H23), C18A(H18A), C19A(H19A), C21A(H21A), C22A(H22A), C23A(H23A)
5.d Fitted hexagon refined as free rotating group:
 C17A(C18A,C19A,C20A,C21A,C22A)
5.e X=CH2 refined with riding coordinates:
 C1(H1A,H1B), C24(H24A,H24B), C24A(H24C,H24D)
;
_shelx_res_checksum              67010
_shelx_hkl_checksum              11130
_olex2_submission_special_instructions 'No special instructions were received'