#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:30:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180224 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/10/7111099.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7111099
loop_
_publ_author_name
'Jouaiti, Abdelaziz'
'Loï, Marielle'
'Hosseini, Mir Wais'
'De Cian, André'
_publ_section_title
;
 Metallacyclophanes formed by a tetrapyrazolyl ligand and copper(ii)
 cation
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2085
_journal_paper_doi               10.1039/b006665f
_journal_year                    2000
_chemical_formula_moiety         'C40 H38 Cl12 Cu3 N16 O2'
_chemical_formula_sum            'C40 H38 Cl12 Cu3 N16 O2'
_chemical_formula_weight         1390.91
_chemical_name_systematic        ' ?'
_space_group_IT_number           71
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2'
_symmetry_space_group_name_H-M   'I m m m'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0302(5)
_cell_length_b                   11.3568(6)
_cell_length_c                   23.5388(7)
_cell_measurement_reflns_used    8320
_cell_measurement_temperature    294
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     2681.3(2)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      294
_diffrn_measurement_details
;
   8320 reflections were collected using program Collect
 ("Collect" Data collection software, Nonius B.V., 1998)
 The conditions were as follow : crystal to detector distance =  36. mm.
 Scan angle =  2.0 deg 1 scans of   40 sec per frame.
 Data collection was divided into  2 set(s)
 with the following starting angles and number of frames :

 Set 1 Theta =    8.20 Omega =    0.00 Kappa =    0.00   79 frames
 Set 2 Theta =   -6.40 Kappa =  172.00 Phi   =    0.00   14 frames
 Friedel pairs were not averaged. Internal R = 0.03
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'π scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            8320
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.830
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.72
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             1394
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.810
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.285
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1486
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.050
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo²/(σ²(Fo²)+0.0001 Fo⁴)+0.5'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.064
_refine_ls_wR_factor_ref         0.052
_reflns_number_gt                1486
_reflns_number_total             1739
_reflns_threshold_expression     >3.0σ(I)
_cod_data_source_file            b006665fsup1.cif
_cod_data_source_block           st517
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^)+0.0001
Fo^4^)+0.5' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0001 Fo^4^)+0.5'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2681.3(4)
_cod_database_code               7111099
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,+z
-x,+y,-z
+x,-y,-z
-x,-y,-z
+x,+y,-z
+x,-y,+z
-x,+y,+z
1/2+x,1/2+y,1/2+z
1/2-x,1/2-y,1/2+z
1/2-x,1/2+y,1/2-z
1/2+x,1/2-y,1/2-z
1/2-x,1/2-y,1/2-z
1/2+x,1/2+y,1/2-z
1/2+x,1/2-y,1/2+z
1/2-x,1/2+y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
CU1 0.5000 0.0000 0.15765(3) 0.0111(3) 0.250 Uani ? ? Cu
CL1 0.5000 0.0000 0.26154(7) 0.0183(7) 0.250 Uani ? ? Cl
N1 0.6379(3) -0.1268(2) 0.1474(1) 0.014(1) 1.000 Uani ? ? N
C1 0.7323(4) -0.1607(3) 0.1836(1) 0.019(2) 1.000 Uani ? ? C
C2 0.8049(3) -0.2562(3) 0.1620(1) 0.020(2) 1.000 Uani ? ? C
C3 0.7497(3) -0.2798(3) 0.1099(1) 0.019(1) 1.000 Uani ? ? C
N2 0.6479(3) -0.2018(2) 0.1020(1) 0.013(1) 1.000 Uani ? ? N
C4 0.5700(3) -0.1897(3) 0.0514(1) 0.013(1) 1.000 Uani ? ? C
C5 0.6381(5) -0.1871(4) 0.0000 0.014(2) 0.500 Uani ? ? C
CU2 1.0000 -0.5000 0.0000 0.0250(6) 0.125 Uani ? ? Cu
CL2 0.7726(2) -0.5000 0.0000 0.0234(8) 0.250 Uani ? ? Cl
CL3 1.0000 -0.2990(2) 0.0000 0.032(1) 0.250 Uani ? ? Cl
C6 1.0000 0.0000 0.0900(6) 0.080(9) 0.250 Uani ? ? C
O 0.879(2) 0.0000 0.0597(5) 0.078(8) 0.250 Uani ? ? O
C7 0.445(1) -0.5000 0.1780(5) 0.027(5) 0.250 Uani ? ? C
CL4 0.5000 -0.5000 0.10774(9) 0.037(1) 0.250 Uani ? ? Cl
CL5 0.5000 -0.3724(1) 0.21452(6) 0.0342(7) 0.500 Uani ? ? Cl
H1 0.7484 -0.1249 0.2194 0.0251 1.000 Uiso calc C1 H
H2 0.8770 -0.2961 0.1798 0.0267 1.000 Uiso calc C2 H
H3 0.7773 -0.3393 0.0841 0.0244 1.000 Uiso calc C3 H
H4 0.7328 -0.1835 0.0000 0.0186 0.500 Uiso calc C5 H
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1
H 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1
Cl 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1
Cu 0.263 1.266 International_Tables_Vol_IV_Table_2.3.1
N 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1
O 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1
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_2
_geom_angle_site_symmetry_3
CL1 CU1 N1 96.90(8) . .
CL1 CU1 N1 96.90(8) . 2_655
CL1 CU1 N1 96.90(8) . 7_555
CL1 CU1 N1 96.90(8) . 8_655
N1 CU1 N1 166.2(2) . 2_655
N1 CU1 N1 91.4(2) . 7_555
N1 CU1 N1 86.9(2) . 8_655
N1 CU1 N1 86.9(2) 2_655 7_555
N1 CU1 N1 91.4(2) 2_655 8_655
N1 CU1 N1 166.2(2) 7_555 8_655
C1 N1 N2 105.5(3) . .
N1 C1 C2 111.3(3) . .
C1 C2 C3 105.4(3) . .
C2 C3 N2 107.3(3) . .
N1 N2 C3 110.6(3) . .
N1 N2 C4 123.3(3) . .
C3 N2 C4 125.8(3) . .
N2 C4 C4 123.1(2) . 8_655
N2 C4 C5 117.3(3) . .
C4 C4 C5 119.4(2) 8_655 .
C4 C5 C4 121.1(4) . 6_555
CL2 CU2 CL2 180.00 . 5_745
CL2 CU2 CL3 90.00 . .
CL2 CU2 CL3 90.00 . 5_745
CL2 CU2 CL3 90.00 5_745 .
CL2 CU2 CL3 90.00 5_745 5_745
CL3 CU2 CL3 180.00 . 5_745
C7 C7 CL4 71.7(4) 2_645 .
C7 C7 CL5 72.0(4) 2_645 .
C7 C7 CL5 72.0(4) 2_645 2_645
CL4 C7 CL5 111.3(4) . .
CL4 C7 CL5 111.3(4) . 2_645
CL5 C7 CL5 109.8(6) . 2_645
C7 CL4 C7 36.7(8) . 2_645
C7 CL5 C7 36.1(7) . 2_645
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
CU1 CL1 2.445(2) .
CU1 CL1 2.445(2) 2_655
CU1 CL1 2.445(2) 7_555
CU1 CL1 2.445(2) 8_655
CU1 N1 2.011(3) .
CU1 N1 2.011(3) 2_655
CU1 N1 2.011(3) 7_555
CU1 N1 2.011(3) 8_655
N1 C1 1.331(4) .
N1 N2 1.371(4) .
C1 C2 1.400(5) .
C2 C3 1.372(5) .
C3 N2 1.365(4) .
N2 C4 1.430(4) .
C4 C4 1.405(6) 8_655
C4 C5 1.391(4) .
C4 C5 1.391(4) 6_555
CU2 CL2 2.281(2) .
CU2 CL2 2.281(2) 5_745
CU2 CL2 2.281(2) 2_745
CU2 CL2 2.281(2) 6_555
CU2 CL2 2.281(2) 3_755
CU2 CL2 2.281(2) 7_545
CU2 CL2 2.281(2) 4_545
CU2 CL2 2.281(2) 8_755
CU2 CL3 2.283(2) .
CU2 CL3 2.283(2) 5_745
CU2 CL3 2.283(2) 2_745
CU2 CL3 2.283(2) 6_555
CU2 CL3 2.283(2) 3_755
CU2 CL3 2.283(2) 7_545
CU2 CL3 2.283(2) 4_545
CU2 CL3 2.283(2) 8_755
C7 C7 1.10(2) 2_645
C7 C7 1.10(2) 8_655
C7 CL4 1.74(1) .
C7 CL4 1.74(1) 2_645
C7 CL4 1.74(1) 7_545
C7 CL4 1.74(1) 8_655
C7 CL5 1.772(7) .
C7 CL5 1.772(7) 2_645
C7 CL5 1.772(7) 7_545
C7 CL5 1.772(7) 8_655
