#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:22:36 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180075 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/21/7052157.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_7052157
loop_
_publ_author_name
'Liliana Dobrzańska'
'Gareth O. Lloyd'
'Leonard J. Barbour'
_publ_section_title
;
 The solvent-templating effect as the driving factor that influences
 the formation of crystalline materials based on the stacking of
 metallocycles
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              669
_journal_paper_doi               10.1039/b618495m
_journal_volume                  31
_journal_year                    2007
_chemical_formula_moiety         'C32 H36 Cl4 Cu2 N8, C3 H3 Cl9'
_chemical_formula_sum            'C35 H39 Cl13 Cu2 N8'
_chemical_formula_weight         1159.67
_chemical_name_common            7
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 121.048(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.700(13)
_cell_length_b                   21.205(18)
_cell_length_c                   8.132(7)
_cell_measurement_temperature    173(2)
_cell_volume                     2319(3)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'X-Seed (Barbour 2001)'
_computing_publication_material  'X-Seed (Barbour 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1316
_diffrn_reflns_av_sigmaI/netI    0.2080
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            4230
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_T_max  0.7269
_exptl_absorpt_correction_T_min  0.6290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            reddish-brown
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.814
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2043
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1739
_refine_ls_R_factor_gt           0.0824
_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/[σ²(Fo²)+(0.0943P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1724
_refine_ls_wR_factor_ref         0.2169
_reflns_number_gt                1016
_reflns_number_total             2043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b618495m.txt
_cod_data_source_block           6
_cod_original_cell_volume        2320(4)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7052157
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.23430(9) 0.0000 0.0203(5) Uani 1 2 d S . .
Cl1 Cl -0.05294(18) 0.28521(13) -0.2836(4) 0.0271(7) Uani 1 1 d . . .
N1 N 0.1307(6) 0.2048(4) 0.0528(12) 0.018(2) Uani 1 1 d . . .
Cl2 Cl -0.0054(3) 0.0000 0.2696(8) 0.0464(13) Uani 1 2 d S . .
C2 C 0.1567(7) 0.1801(5) -0.0655(15) 0.019(2) Uani 1 1 d . . .
Cl3 Cl 0.1763(2) 0.06895(14) 0.3909(5) 0.0384(8) Uani 1 1 d . . .
N3 N 0.2554(6) 0.1669(4) 0.0308(12) 0.021(2) Uani 1 1 d . . .
Cl4 Cl 0.4638(4) -0.0686(3) 0.5665(9) 0.0361(15) Uani 0.50 1 d PD . .
C4 C 0.2960(7) 0.1852(4) 0.2202(15) 0.020(2) Uani 1 1 d . . .
H4 H 0.3636 0.1826 0.3208 0.024 Uiso 1 1 calc R . .
Cl5 Cl 0.5970(6) 0.0000 0.4863(13) 0.038(2) Uani 0.50 2 d SPD . .
C5 C 0.2171(7) 0.2080(5) 0.2304(16) 0.025(3) Uani 1 1 d . . .
H5 H 0.2213 0.2238 0.3436 0.030 Uiso 1 1 calc R . .
C6 C 0.0913(7) 0.1645(5) -0.2674(15) 0.023(3) Uani 1 1 d . . .
H6A H 0.0219 0.1677 -0.3007 0.035 Uiso 1 1 calc R . .
H6B H 0.1049 0.1214 -0.2907 0.035 Uiso 1 1 calc R . .
H6C H 0.1030 0.1939 -0.3466 0.035 Uiso 1 1 calc R . .
C7 C 0.3117(7) 0.1371(4) -0.0469(16) 0.021(3) Uani 1 1 d . . .
H7A H 0.3819 0.1508 0.0299 0.026 Uiso 1 1 calc R . .
H7B H 0.2848 0.1519 -0.1803 0.026 Uiso 1 1 calc R . .
C8 C 0.3078(7) 0.0657(5) -0.0462(15) 0.022(3) Uani 1 1 d . . .
C9 C 0.2529(7) 0.0322(5) 0.0154(16) 0.020(2) Uani 1 1 d . . .
H9 H 0.2152 0.0544 0.0579 0.025 Uiso 1 1 calc R . .
C10 C 0.3622(8) 0.0318(5) -0.1070(18) 0.029(3) Uani 1 1 d . . .
H10 H 0.4001 0.0537 -0.1494 0.035 Uiso 1 1 calc R . .
C11 C 0.1243(11) 0.0000 0.429(3) 0.029(4) Uani 1 2 d S . .
H11 H 0.1386 0.0000 0.5638 0.035 Uiso 1 2 calc SR . .
C12 C 0.4778(8) 0.0000 0.459(2) 0.021(7) Uiso 0.50 2 d SPD . .
H12 H 0.4261 0.0000 0.3191 0.025 Uiso 0.50 2 calc SPR . .
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'
Cl Cl 0.1484 0.1585 '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'
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 Cu1 N1 143.0(5) . 2 ?
N1 Cu1 Cl1 97.7(3) . 2 ?
N1 Cu1 Cl1 99.6(3) 2 2 ?
N1 Cu1 Cl1 99.6(3) . . ?
N1 Cu1 Cl1 97.7(3) 2 . ?
Cl1 Cu1 Cl1 123.47(18) 2 . ?
C2 N1 C5 105.8(8) . . ?
C2 N1 Cu1 129.9(7) . . ?
C5 N1 Cu1 124.3(7) . . ?
N1 C2 N3 110.4(9) . . ?
N1 C2 C6 127.1(9) . . ?
N3 C2 C6 122.4(10) . . ?
C2 N3 C4 108.6(9) . . ?
C2 N3 C7 127.0(9) . . ?
C4 N3 C7 124.4(8) . . ?
Cl5 Cl4 C12 49.9(5) 5_656 . ?
Cl5 Cl4 C12 61.4(3) 5_656 5_656 ?
C12 Cl4 C12 21.8(9) . 5_656 ?
Cl5 Cl4 Cl4 106.3(4) 5_656 2_656 ?
C12 Cl4 Cl4 57.6(3) . 2_656 ?
C12 Cl4 Cl4 56.6(4) 5_656 2_656 ?
C5 C4 N3 104.7(8) . . ?
C12 Cl5 Cl4 68.5(4) 5_656 2_656 ?
C12 Cl5 Cl4 68.5(4) 5_656 5_656 ?
Cl4 Cl5 Cl4 121.2(6) 2_656 5_656 ?
C12 Cl5 C12 21.4(11) 5_656 . ?
Cl4 Cl5 C12 62.6(3) 2_656 . ?
Cl4 Cl5 C12 62.6(3) 5_656 . ?
C4 C5 N1 110.5(10) . . ?
N3 C7 C8 113.2(8) . . ?
C10 C8 C9 118.1(10) . . ?
C10 C8 C7 118.9(9) . . ?
C9 C8 C7 123.0(10) . . ?
C9 C9 C8 120.6(6) 6 . ?
C10 C10 C8 121.2(6) 6 . ?
Cl2 C11 Cl3 109.4(7) . . ?
Cl2 C11 Cl3 109.4(7) . 6 ?
Cl3 C11 Cl3 110.7(8) . 6 ?
Cl5 C12 Cl4 109.4(5) . 6 ?
Cl5 C12 Cl4 109.4(5) . . ?
Cl4 C12 Cl4 110.7(8) 6 . ?
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
Cu1 N1 1.970(8) . ?
Cu1 N1 1.970(8) 2 ?
Cu1 Cl1 2.280(3) 2 ?
Cu1 Cl1 2.280(3) . ?
N1 C2 1.331(13) . ?
N1 C5 1.382(12) . ?
Cl2 C11 1.761(16) . ?
C2 N3 1.356(12) . ?
C2 C6 1.456(13) . ?
Cl3 C11 1.778(9) . ?
N3 C4 1.384(13) . ?
N3 C7 1.469(13) . ?
Cl4 Cl5 1.671(7) 5_656 ?
Cl4 C12 1.769(5) . ?
Cl4 C12 1.789(9) 5_656 ?
Cl4 Cl4 1.931(12) 2_656 ?
C4 C5 1.371(14) . ?
Cl5 C12 1.455(14) 5_656 ?
Cl5 Cl4 1.671(7) 2_656 ?
Cl5 Cl4 1.671(7) 5_656 ?
Cl5 C12 1.768(5) . ?
C7 C8 1.516(14) . ?
C8 C10 1.389(15) . ?
C8 C9 1.393(14) . ?
C9 C9 1.367(19) 6 ?
C10 C10 1.35(2) 6 ?
C11 Cl3 1.778(9) 6 ?
C12 Cl4 1.769(5) 6 ?
