#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/21/8102153.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_8102153
loop_
_publ_author_name
'Glatz, Germund'
'Irrgang, Torsten'
'Kempe, Rhett'
_publ_section_title
;
Crystal structure of bis(μ-bromo)-tetrakis(tert-butyl-(4-methyl-
pyridin-2-yl)-amine)-dicopper(I), Cu₂Br₂(C₁₀H₁₆N₂)₄
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              287
_journal_page_last               288
_journal_volume                  222
_journal_year                    2007
_chemical_formula_structural     Cu2Br2(C10H16N2)4
_chemical_formula_sum            'C40 H64 Br2 Cu2 N8'
_chemical_formula_weight         943.89
_chemical_name_systematic
;
bis(μ-bromo)-tetrakis(tert-butyl-(4-methyl-pyridin-2-yl)-amine)-dicopper(I)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.604(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3890(7)
_cell_length_b                   16.5070(8)
_cell_length_c                   23.7280(19)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    191(2)
_cell_volume                     4431.2(5)
_computing_data_collection       X-AREA-STOE
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      191(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0752
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7862
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    2.800
_exptl_absorpt_correction_T_max  0.6869
_exptl_absorpt_correction_T_min  0.4433
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          1.077
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0379P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0806
_reflns_number_gt                2654
_reflns_number_total             4150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2048.cff
_cod_data_source_block           k384m
_cod_original_sg_symbol_H-M      C12/c1
_cod_database_code               8102153
#BEGIN Tags that were not found in dictionaries:
_cell_measurement_2theta_min     3.45
_cell_measurement_2theta_max     51.96
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8943(4) 0.8414(3) 0.18569(16) 0.0412(11) Uani 1 8 f d . . .
H1 H 0.8294 0.8747 0.1925 0.049 Uiso 1 8 f calc R . .
C2 C 0.8756(4) 0.7599(3) 0.18148(16) 0.0441(11) Uani 1 8 f d . . .
H2 H 0.7999 0.7377 0.1853 0.053 Uiso 1 8 f calc R . .
C3 C 0.9689(4) 0.7101(3) 0.17156(16) 0.0390(10) Uani 1 8 f d . . .
C4 C 1.0757(4) 0.7455(2) 0.16642(16) 0.0367(10) Uani 1 8 f d . . .
H4 H 1.1410 0.7126 0.1595 0.044 Uiso 1 8 f calc R . .
C5 C 1.0901(4) 0.8295(2) 0.17115(15) 0.0347(9) Uani 1 8 f d . . .
C6 C 1.3114(4) 0.8361(3) 0.16395(19) 0.0448(11) Uani 1 8 f d . . .
C7 C 1.3936(4) 0.9088(3) 0.1667(2) 0.0604(14) Uani 1 8 f d . . .
H7A H 1.3693 0.9452 0.1348 0.091 Uiso 1 8 f calc R . .
H7B H 1.4748 0.8904 0.1645 0.091 Uiso 1 8 f calc R . .
H7C H 1.3898 0.9377 0.2025 0.091 Uiso 1 8 f calc R . .
C8 C 1.3505(4) 0.7798(3) 0.2136(2) 0.0655(15) Uani 1 8 f d . . .
H8A H 1.3531 0.8101 0.2493 0.098 Uiso 1 8 f calc R . .
H8B H 1.4293 0.7583 0.2096 0.098 Uiso 1 8 f calc R . .
H8C H 1.2942 0.7349 0.2140 0.098 Uiso 1 8 f calc R . .
C9 C 1.3177(5) 0.7923(3) 0.1077(2) 0.0660(15) Uani 1 8 f d . . .
H9A H 1.2682 0.7436 0.1063 0.099 Uiso 1 8 f calc R . .
H9B H 1.3997 0.7769 0.1044 0.099 Uiso 1 8 f calc R . .
H9C H 1.2891 0.8284 0.0763 0.099 Uiso 1 8 f calc R . .
C10 C 0.9539(5) 0.6197(3) 0.1681(2) 0.0557(13) Uani 1 8 f d . . .
H10A H 0.9178 0.6048 0.1300 0.084 Uiso 1 8 f calc R . .
H10B H 0.9029 0.6019 0.1963 0.084 Uiso 1 8 f calc R . .
H10C H 1.0314 0.5936 0.1757 0.084 Uiso 1 8 f calc R . .
C11 C 1.0995(4) 1.1304(3) 0.12470(17) 0.0438(11) Uani 1 8 f d . . .
H11 H 1.1550 1.1344 0.1577 0.053 Uiso 1 8 f calc R . .
C12 C 1.1131(4) 1.1818(3) 0.08022(18) 0.0489(12) Uani 1 8 f d . . .
H12 H 1.1744 1.2211 0.0830 0.059 Uiso 1 8 f calc R . .
C13 C 1.0351(4) 1.1744(3) 0.03148(17) 0.0477(12) Uani 1 8 f d . . .
C14 C 0.9469(4) 1.1185(3) 0.03018(17) 0.0482(12) Uani 1 8 f d . . .
H14 H 0.8928 1.1126 -0.0032 0.058 Uiso 1 8 f calc R . .
C15 C 0.9349(4) 1.0693(3) 0.07778(17) 0.0460(11) Uani 1 8 f d . . .
C16 C 0.7306(4) 1.0080(3) 0.04810(18) 0.0506(12) Uani 1 8 f d . . .
C17 C 0.7391(5) 0.9786(3) -0.0120(2) 0.0704(16) Uani 1 8 f d . . .
H17A H 0.7824 1.0185 -0.0322 0.106 Uiso 1 8 f calc R . .
H17B H 0.6594 0.9716 -0.0318 0.106 Uiso 1 8 f calc R . .
H17C H 0.7810 0.9267 -0.0107 0.106 Uiso 1 8 f calc R . .
C18 C 0.6651(5) 0.9447(4) 0.0789(2) 0.0746(17) Uani 1 8 f d . . .
H18A H 0.7087 0.8935 0.0802 0.112 Uiso 1 8 f calc R . .
H18B H 0.5859 0.9367 0.0588 0.112 Uiso 1 8 f calc R . .
H18C H 0.6585 0.9632 0.1177 0.112 Uiso 1 8 f calc R . .
C19 C 0.6674(5) 1.0883(3) 0.0476(2) 0.0670(15) Uani 1 8 f d . . .
H19A H 0.6651 1.1069 0.0867 0.101 Uiso 1 8 f calc R . .
H19B H 0.5866 1.0820 0.0290 0.101 Uiso 1 8 f calc R . .
H19C H 0.7095 1.1281 0.0268 0.101 Uiso 1 8 f calc R . .
C20 C 1.0488(5) 1.2263(3) -0.0199(2) 0.0704(16) Uani 1 8 f d . . .
H20A H 1.0453 1.1919 -0.0537 0.106 Uiso 1 8 f calc R . .
H20B H 1.1251 1.2543 -0.0144 0.106 Uiso 1 8 f calc R . .
H20C H 0.9848 1.2662 -0.0248 0.106 Uiso 1 8 f calc R . .
N1 N 0.9984(3) 0.8778(2) 0.18092(12) 0.0362(8) Uani 1 8 f d . . .
N2 N 1.1936(3) 0.8691(2) 0.16730(17) 0.0482(10) Uani 1 8 f d . . .
N3 N 1.0134(3) 1.0752(2) 0.12470(13) 0.0390(8) Uani 1 8 f d . . .
N4 N 0.8493(4) 1.0128(3) 0.0799(2) 0.0681(15) Uani 1 8 f d . . .
Cu1 Cu 1.01025(5) 0.99989(3) 0.19253(2) 0.04087(15) Uani 1 8 f d . . .
Br1 Br 1.18162(4) 1.04016(3) 0.264189(17) 0.04020(13) Uani 1 8 f d . . .
H2N H 1.193(3) 0.916(3) 0.1808(15) 0.029(11) Uiso 1 8 f d . . .
H4N H 0.850(4) 0.996(3) 0.106(2) 0.047(16) Uiso 1 8 f d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 124.5(4) . . ?
C1 C2 C3 118.7(4) . . ?
C4 C3 C2 118.0(4) . . ?
C4 C3 C10 121.0(4) . . ?
C2 C3 C10 120.9(4) . . ?
C3 C4 C5 120.9(4) . . ?
N1 C5 N2 114.8(4) . . ?
N1 C5 C4 120.8(4) . . ?
N2 C5 C4 124.4(4) . . ?
N2 C6 C7 105.6(4) . . ?
N2 C6 C8 111.9(4) . . ?
C7 C6 C8 108.9(4) . . ?
N2 C6 C9 111.1(4) . . ?
C7 C6 C9 108.7(4) . . ?
C8 C6 C9 110.4(4) . . ?
N3 C11 C12 124.5(4) . . ?
C11 C12 C13 118.0(4) . . ?
C14 C13 C12 118.7(4) . . ?
C14 C13 C20 120.6(4) . . ?
C12 C13 C20 120.6(5) . . ?
C13 C14 C15 120.8(4) . . ?
N3 C15 N4 115.6(4) . . ?
N3 C15 C14 120.2(4) . . ?
N4 C15 C14 124.2(4) . . ?
N4 C16 C19 111.5(4) . . ?
N4 C16 C17 110.1(4) . . ?
C19 C16 C17 110.8(4) . . ?
N4 C16 C18 105.3(4) . . ?
C19 C16 C18 110.3(4) . . ?
C17 C16 C18 108.7(4) . . ?
C1 N1 C5 117.1(4) . . ?
C1 N1 Cu1 118.5(3) . . ?
C5 N1 Cu1 124.4(3) . . ?
C5 N2 C6 129.4(4) . . ?
C11 N3 C15 117.7(4) . . ?
C11 N3 Cu1 119.7(3) . . ?
C15 N3 Cu1 122.5(3) . . ?
C15 N4 C16 129.9(5) . . ?
N1 Cu1 N3 120.26(13) . . ?
N1 Cu1 Br1 112.69(9) . . ?
N3 Cu1 Br1 106.78(10) . . ?
N1 Cu1 Br1 105.08(10) . 2_755 ?
N3 Cu1 Br1 104.34(10) . 2_755 ?
Br1 Cu1 Br1 106.60(2) . 2_755 ?
N1 Cu1 Cu1 96.99(8) . 2_755 ?
N3 Cu1 Cu1 142.26(10) . 2_755 ?
Br1 Cu1 Cu1 58.81(2) . 2_755 ?
Br1 Cu1 Cu1 56.02(2) 2_755 2_755 ?
Cu1 Br1 Cu1 65.16(2) . 2_755 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.345(5) . ?
C1 C2 1.364(6) . ?
C2 C3 1.385(6) . ?
C3 C4 1.367(6) . ?
C3 C10 1.503(6) . ?
C4 C5 1.400(5) . ?
C5 N1 1.355(5) . ?
C5 N2 1.360(5) . ?
C6 N2 1.459(6) . ?
C6 C7 1.518(6) . ?
C6 C8 1.527(6) . ?
C6 C9 1.527(6) . ?
C11 N3 1.339(5) . ?
C11 C12 1.377(6) . ?
C12 C13 1.380(6) . ?
C13 C14 1.362(6) . ?
C13 C20 1.511(6) . ?
C14 C15 1.411(6) . ?
C15 N3 1.349(5) . ?
C15 N4 1.354(6) . ?
C16 N4 1.472(6) . ?
C16 C19 1.508(7) . ?
C16 C17 1.519(6) . ?
C16 C18 1.519(7) . ?
N1 Cu1 2.037(3) . ?
N3 Cu1 2.037(3) . ?
Cu1 Br1 2.5257(7) . ?
Cu1 Br1 2.6054(7) 2_755 ?
Cu1 Cu1 2.7640(10) 2_755 ?
Br1 Cu1 2.6054(7) 2_755 ?
