#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:25:42 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179843 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/39/7013943.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_7013943
loop_
_publ_author_name
'Solntsev, Pavlo V.'
'Sieler, Joachim'
'Krautscheid, Harald'
'Domasevitch, Konstantin V.'
_publ_section_title
;
 Fused pyridazines: rigid multidentates for designing and fine-tuning
 the structure of hybrid organic/inorganic frameworks.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1153
_journal_page_last               1158
_journal_paper_doi               10.1039/b316561b
_journal_year                    2004
_chemical_formula_sum            'C80 H84 Cu18 I18 N28'
_chemical_formula_weight         4865.67
_chemical_name_common
;
Copper(i) Iodide 3:1 Complex with 1,2,3,6,7,8-Hexahydro-
cinnolino(5,4,3-cde)cinnoline, acetonitrile solvate
;
_chemical_name_systematic
;
Copper(I) Iodide 3:1 Complex with
1,2,3,6,7,8-Hexahydro-cinnolino[5,4,3-cde]cinnoline, acetonitrile solvate
;
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   20.463(2)
_cell_length_b                   20.463(2)
_cell_length_c                   17.989(2)
_cell_measurement_temperature    223(2)
_cell_volume                     6523.4(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'omega scans'
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38755
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    7.171
_exptl_absorpt_correction_T_max  0.2672
_exptl_absorpt_correction_T_min  0.1407
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             4472
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.262
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0310P)²+62.2325P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                2417
_reflns_number_total             2792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b316561b.txt
_cod_data_source_block           c1552
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+62.2325P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+62.2325P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6523.6(12)
_cod_original_sg_symbol_H-M      P6(3)/mmc
_cod_database_code               7013943
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.09222(4) 0.34004(4) 0.48494(3) 0.02075(17) Uani 1 d . . .
Cu2 Cu 0.59578(6) 0.19155(12) 0.7500 0.0475(5) Uani 1 d S . .
Cu3 Cu -0.12343(7) 0.12343(7) 0.42372(13) 0.0372(5) Uani 0.50 d SP . .
I1 I 0.0000 0.19454(3) 0.5000 0.02935(16) Uani 1 d S . .
I2 I 0.194888(17) 0.38978(3) 0.59218(3) 0.03047(17) Uani 1 d S . .
I3 I 0.52485(5) 0.26242(3) 0.7500 0.0426(2) Uani 1 d S . .
I4 I 0.52490(4) 0.04981(8) 0.7500 0.0704(4) Uani 1 d S . .
N1 N 0.1358(2) 0.3398(2) 0.3820(2) 0.0165(8) Uani 1 d . . .
N2 N 0.0377(2) 0.4019(2) 0.4894(2) 0.0170(8) Uani 1 d . . .
N3 N -0.0976(8) 0.0976(8) 0.3221(8) 0.061(6) Uani 0.50 d SP . .
C1 C 0.0997(3) 0.3326(3) 0.3189(3) 0.0181(9) Uani 1 d . . .
C2 C 0.1311(4) 0.3292(4) 0.2500 0.0182(13) Uani 1 d S . .
C3 C 0.0264(3) 0.3330(4) 0.3208(3) 0.0249(11) Uani 1 d . . .
H3A H 0.0365 0.3841 0.3244 0.080 Uiso 1 d R . .
H3B H -0.0020 0.3060 0.3638 0.080 Uiso 1 d R . .
C4 C -0.0198(4) 0.2962(6) 0.2500 0.0273(17) Uani 1 d S . .
H4A H -0.0642 0.3009 0.2500 0.080 Uiso 1 d SR . .
H4B H -0.0356 0.2435 0.2500 0.080 Uiso 1 d SR . .
C5 C 0.0738(3) 0.4762(3) 0.4775(3) 0.0190(9) Uani 1 d . . .
C6 C 0.0372(4) 0.51859(19) 0.4880(4) 0.0171(13) Uani 1 d S . .
C7 C 0.1540(3) 0.5148(3) 0.4510(4) 0.0307(13) Uani 1 d . . .
H7A H 0.1546 0.5093 0.3980 0.080 Uiso 1 d R . .
H7B H 0.1794 0.4909 0.4730 0.080 Uiso 1 d R . .
C8 C 0.1957(5) 0.5978(3) 0.4707(7) 0.042(2) Uani 1 d S . .
H8A H 0.2435 0.6218 0.4456 0.080 Uiso 1 d SR . .
H8B H 0.2055 0.6028 0.5232 0.080 Uiso 1 d SR . .
C9 C -0.0904(8) 0.0904(8) 0.2500 0.084(7) Uani 1 d S . .
N4 N 0.0000 0.0000 0.289(4) 0.101(17) Uiso 0.50 d SP . .
C10 C 0.0000 0.0000 0.349(5) 0.10(2) Uiso 0.50 d SP . .
C11 C 0.0000 0.0000 0.440(5) 0.092(19) Uiso 0.50 d SP . .
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'
I I -0.4742 1.8119 '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 N2 113.86(16) . . ?
N1 Cu1 I1 99.04(12) . . ?
N2 Cu1 I1 112.90(12) . . ?
N1 Cu1 I2 113.23(12) . . ?
N2 Cu1 I2 107.67(12) . . ?
I1 Cu1 I2 110.04(3) . . ?
N1 Cu1 Cu3 106.12(12) . 14_556 ?
N2 Cu1 Cu3 139.96(12) . 14_556 ?
I1 Cu1 Cu3 56.65(5) . 14_556 ?
I2 Cu1 Cu3 55.40(5) . 14_556 ?
I4 Cu2 I3 119.99(5) . 2_655 ?
I4 Cu2 I3 119.99(5) . . ?
I3 Cu2 I3 120.02(9) 2_655 . ?
N3 Cu3 I2 110.1(7) . 15_556 ?
N3 Cu3 I1 108.3(4) . . ?
I2 Cu3 I1 114.54(6) 15_556 . ?
N3 Cu3 I1 108.3(4) . 15_556 ?
I2 Cu3 I1 114.54(6) 15_556 15_556 ?
I1 Cu3 I1 100.48(8) . 15_556 ?
N3 Cu3 Cu1 141.5(3) . 9_556 ?
I2 Cu3 Cu1 58.92(5) 15_556 9_556 ?
I1 Cu3 Cu1 57.81(4) . 9_556 ?
I1 Cu3 Cu1 109.55(8) 15_556 9_556 ?
N3 Cu3 Cu1 141.5(3) . 15_556 ?
I2 Cu3 Cu1 58.92(5) 15_556 15_556 ?
I1 Cu3 Cu1 109.55(8) . 15_556 ?
I1 Cu3 Cu1 57.81(4) 15_556 15_556 ?
Cu1 Cu3 Cu1 68.70(6) 9_556 15_556 ?
Cu3 I1 Cu3 171.48(10) . 14_556 ?
Cu3 I1 Cu1 121.95(5) . . ?
Cu3 I1 Cu1 65.55(6) 14_556 . ?
Cu3 I1 Cu1 65.55(6) . 9_556 ?
Cu3 I1 Cu1 121.95(5) 14_556 9_556 ?
Cu1 I1 Cu1 78.32(3) . 9_556 ?
Cu3 I2 Cu1 65.68(4) 14_556 20 ?
Cu3 I2 Cu1 65.68(4) 14_556 . ?
Cu1 I2 Cu1 73.79(3) 20 . ?
Cu2 I3 Cu2 119.98(9) 3_665 . ?
C1 N1 N1 120.2(3) . 20 ?
C1 N1 Cu1 123.7(3) . . ?
N1 N1 Cu1 115.79(11) 20 . ?
C5 N2 N2 120.4(3) . 9_556 ?
C5 N2 Cu1 122.0(3) . . ?
N2 N2 Cu1 117.43(12) 9_556 . ?
C9 N3 Cu3 165(2) . . ?
N1 C1 C2 121.1(5) . . ?
N1 C1 C3 118.9(4) . . ?
C2 C1 C3 119.8(5) . . ?
C2 C2 C1 118.6(3) 20 16_556 ?
C2 C2 C1 118.6(3) 20 . ?
C1 C2 C1 122.6(6) 16_556 . ?
C1 C3 C4 110.5(5) . . ?
C3 C4 C3 111.5(7) . 16_556 ?
N2 C5 C6 121.0(5) . . ?
N2 C5 C7 119.2(5) . . ?
C6 C5 C7 119.7(5) . . ?
C6 C6 C5 118.5(3) 13_566 . ?
C6 C6 C5 118.5(3) 13_566 21_565 ?
C5 C6 C5 122.9(6) . 21_565 ?
C5 C7 C8 111.7(5) . . ?
C7 C8 C7 114.5(8) 21_565 . ?
N3 C9 N3 158(3) 16_556 . ?
C10 N4 N4 180.000(16) . 16_556 ?
N4 C10 C11 180.00(2) . . ?
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 2.056(4) . ?
Cu1 N2 2.066(4) . ?
Cu1 I1 2.6232(8) . ?
Cu1 I2 2.6521(8) . ?
Cu1 Cu3 2.822(2) 14_556 ?
Cu2 I4 2.512(3) . ?
Cu2 I3 2.5130(12) 2_655 ?
Cu2 I3 2.5130(12) . ?
Cu3 N3 2.04(2) . ?
Cu3 I2 2.549(3) 15_556 ?
Cu3 I1 2.5893(16) . ?
Cu3 I1 2.5893(16) 15_556 ?
Cu3 Cu1 2.822(2) 9_556 ?
Cu3 Cu1 2.822(2) 15_556 ?
I1 Cu3 2.5893(16) 14_556 ?
I1 Cu1 2.6232(8) 9_556 ?
I2 Cu3 2.549(3) 14_556 ?
I2 Cu1 2.6521(8) 20 ?
I3 Cu2 2.5130(12) 3_665 ?
N1 C1 1.322(6) . ?
N1 N1 1.395(8) 20 ?
N2 C5 1.334(6) . ?
N2 N2 1.389(8) 9_556 ?
N3 C9 1.322(17) . ?
C1 C2 1.414(6) . ?
C1 C3 1.504(7) . ?
C2 C2 1.373(14) 20 ?
C2 C1 1.414(6) 16_556 ?
C3 C4 1.540(7) . ?
C4 C3 1.540(7) 16_556 ?
C5 C6 1.415(6) . ?
C5 C7 1.499(7) . ?
C6 C6 1.387(13) 13_566 ?
C6 C5 1.415(6) 21_565 ?
C7 C8 1.514(9) . ?
C8 C7 1.514(8) 21_565 ?
C9 N3 1.322(17) 16_556 ?
N4 C10 1.08(10) . ?
N4 N4 1.42(15) 16_556 ?
C10 C11 1.63(13) . ?
