#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/03/2230363.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2230363
loop_
_publ_author_name
'Wöhlert, Susanne'
'Wriedt, Mario'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Chloridotetrapyridinecopper(II) dicyanamidate pyridine disolvate
;
_journal_coeditor_code           IM2272
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m695
_journal_paper_doi               10.1107/S1600536811016187
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Cu Cl (C5 H5 N)4] (C2 N3), 2C6 H5 N'
_chemical_formula_moiety         'C20 H20 Cl Cu N4 +, C2 N3 -, 2(C5 H5 N)'
_chemical_formula_sum            'C32 H30 Cl Cu N9'
_chemical_formula_weight         639.64
_chemical_name_systematic
;
Chloridotetrapyridinecopper(II) dicyanamidate pyridine disolvate
;
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2859(6)
_cell_length_b                   17.6577(9)
_cell_length_c                   11.4818(9)
_cell_measurement_reflns_used    16623
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.66
_cell_volume                     3099.1(3)
_computing_cell_refinement       'IPDS (Stoe & Cie, 1998)'
_computing_data_collection       'IPDS (Stoe & Cie, 1998)'
_computing_data_reduction        'IPDS (Stoe & Cie, 1998)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'CIFTAB in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       φ
_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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16623
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1998)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.4751
_exptl_crystal_size_mid          0.1797
_exptl_crystal_size_min          0.0776
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.557
_refine_ls_abs_structure_details 'Flack (1983), 1740 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       0.0056(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3708
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0648P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                3220
_reflns_number_total             3708
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            im2272.cif
_cod_data_source_block           I
_cod_database_code               2230363
_cod_database_fobs_code          2230363
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+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1, -y+1, z+1/2'
'-x+1, y+1, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.5000 0.5000 0.78178(3) 0.01901(12) Uani d S 1 2 . .
Cl Cl1 0.5000 0.5000 1.01993(7) 0.01916(17) Uani d S 1 2 . .
N N1 0.51436(10) 0.38455(9) 0.77683(18) 0.0175(3) Uani d . 1 1 . .
C C2 0.49213(17) 0.26597(16) 0.6798(2) 0.0291(6) Uani d . 1 1 . .
H H2 0.4664 0.2383 0.6177 0.035 Uiso calc R 1 1 . .
C C3 0.54374(17) 0.22991(13) 0.7620(2) 0.0310(5) Uani d . 1 1 . .
H H3 0.5538 0.1769 0.7570 0.037 Uiso calc R 1 1 . .
C C4 0.58055(16) 0.27172(12) 0.8518(2) 0.0288(5) Uani d . 1 1 . .
H H4 0.6160 0.2479 0.9091 0.035 Uiso calc R 1 1 . .
C C5 0.56461(14) 0.34873(12) 0.8560(2) 0.0222(4) Uani d . 1 1 . .
H H5 0.5900 0.3775 0.9172 0.027 Uiso calc R 1 1 . .
N N11 0.63287(11) 0.50796(9) 0.77505(18) 0.0169(3) Uani d . 1 1 . .
C C11 0.67644(14) 0.54903(11) 0.8549(2) 0.0193(4) Uani d . 1 1 . .
H H11 0.6440 0.5768 0.9112 0.023 Uiso calc R 1 1 . .
C C12 0.76675(16) 0.55225(14) 0.8580(2) 0.0257(5) Uani d . 1 1 . .
H H12 0.7960 0.5824 0.9144 0.031 Uiso calc R 1 1 . .
C C13 0.81395(14) 0.51051(14) 0.7770(3) 0.0294(5) Uani d . 1 1 . .
H H13 0.8761 0.5114 0.7777 0.035 Uiso calc R 1 1 . .
C C14 0.76982(15) 0.46773(14) 0.6956(2) 0.0264(5) Uani d . 1 1 . .
H H14 0.8010 0.4386 0.6397 0.032 Uiso calc R 1 1 . .
C C15 0.67906(14) 0.46793(13) 0.6968(2) 0.0210(4) Uani d . 1 1 . .
H H15 0.6485 0.4388 0.6404 0.025 Uiso calc R 1 1 . .
C C1 0.47896(16) 0.34335(13) 0.6904(2) 0.0225(4) Uani d . 1 1 . .
H H1 0.4435 0.3683 0.6342 0.027 Uiso calc R 1 1 . .
N N21 0.79940(15) 0.79986(11) 0.5241(2) 0.0355(5) Uani d . 1 1 . .
C C21 0.7555(2) 0.75937(16) 0.6032(2) 0.0369(6) Uani d . 1 1 . .
H H21 0.7249 0.7859 0.6625 0.044 Uiso calc R 1 1 . .
C C22 0.7521(2) 0.68134(18) 0.6039(3) 0.0413(7) Uani d . 1 1 . .
H H22 0.7193 0.6552 0.6615 0.050 Uiso calc R 1 1 . .
C C23 0.79745(19) 0.64167(15) 0.5190(3) 0.0444(7) Uani d . 1 1 . .
H H23 0.7970 0.5879 0.5178 0.053 Uiso calc R 1 1 . .
C C24 0.8428(2) 0.68182(16) 0.4368(3) 0.0401(7) Uani d . 1 1 . .
H H24 0.8741 0.6566 0.3767 0.048 Uiso calc R 1 1 . .
C C25 0.8419(2) 0.75980(16) 0.4435(3) 0.0378(6) Uani d . 1 1 . .
H H25 0.8740 0.7870 0.3864 0.045 Uiso calc R 1 1 . .
N N30 0.93807(17) 0.38709(14) 0.5329(4) 0.0628(8) Uani d . 1 1 . .
C C30 0.96901(19) 0.44145(16) 0.5161(4) 0.0527(9) Uani d . 1 1 . .
N N31 1.0000 0.5000 0.4511(5) 0.0835(19) Uani d S 1 2 . .
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N11 Cu1 N11 . 2_665 175.66(12) ?
N11 Cu1 N1 . . 87.76(6) ?
N11 Cu1 N1 2_665 . 92.12(6) ?
N11 Cu1 N1 . 2_665 92.12(6) ?
N11 Cu1 N1 2_665 2_665 87.76(6) ?
N1 Cu1 N1 . 2_665 176.83(12) ?
N11 Cu1 Cl1 . . 92.17(6) ?
N11 Cu1 Cl1 2_665 . 92.17(6) ?
N1 Cu1 Cl1 . . 91.59(6) ?
N1 Cu1 Cl1 2_665 . 91.59(6) ?
C1 N1 C5 . . 118.27(18) ?
C1 N1 Cu1 . . 121.01(15) ?
C5 N1 Cu1 . . 120.58(15) ?
C3 C2 C1 . . 118.4(2) ?
C3 C2 H2 . . 120.8 ?
C1 C2 H2 . . 120.8 ?
C2 C3 C4 . . 119.5(2) ?
C2 C3 H3 . . 120.2 ?
C4 C3 H3 . . 120.2 ?
C5 C4 C3 . . 118.6(2) ?
C5 C4 H4 . . 120.7 ?
C3 C4 H4 . . 120.7 ?
N1 C5 C4 . . 122.5(2) ?
N1 C5 H5 . . 118.7 ?
C4 C5 H5 . . 118.7 ?
C15 N11 C11 . . 118.64(17) ?
C15 N11 Cu1 . . 120.85(14) ?
C11 N11 Cu1 . . 120.31(15) ?
N11 C11 C12 . . 122.3(2) ?
N11 C11 H11 . . 118.9 ?
C12 C11 H11 . . 118.9 ?
C11 C12 C13 . . 118.7(2) ?
C11 C12 H12 . . 120.7 ?
C13 C12 H12 . . 120.7 ?
C14 C13 C12 . . 119.39(19) ?
C14 C13 H13 . . 120.3 ?
C12 C13 H13 . . 120.3 ?
C13 C14 C15 . . 118.8(2) ?
C13 C14 H14 . . 120.6 ?
C15 C14 H14 . . 120.6 ?
N11 C15 C14 . . 122.2(2) ?
N11 C15 H15 . . 118.9 ?
C14 C15 H15 . . 118.9 ?
N1 C1 C2 . . 122.6(2) ?
N1 C1 H1 . . 118.7 ?
C2 C1 H1 . . 118.7 ?
C25 N21 C21 . . 115.6(2) ?
N21 C21 C22 . . 123.9(3) ?
N21 C21 H21 . . 118.1 ?
C22 C21 H21 . . 118.1 ?
C21 C22 C23 . . 118.8(2) ?
C21 C22 H22 . . 120.6 ?
C23 C22 H22 . . 120.6 ?
C24 C23 C22 . . 118.4(2) ?
C24 C23 H23 . . 120.8 ?
C22 C23 H23 . . 120.8 ?
C23 C24 C25 . . 118.3(3) ?
C23 C24 H24 . . 120.9 ?
C25 C24 H24 . . 120.9 ?
N21 C25 C24 . . 125.0(2) ?
N21 C25 H25 . . 117.5 ?
C24 C25 H25 . . 117.5 ?
N30 C30 N31 . . 156.9(5) ?
C30 N31 C30 2_765 . 113.5(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N11 . 2.0374(16) ?
Cu1 N11 2_665 2.0374(16) ?
Cu1 N1 . 2.0511(16) ?
Cu1 N1 2_665 2.0511(16) ?
Cu1 Cl1 . 2.7344(9) ?
N1 C1 . 1.345(3) ?
N1 C5 . 1.348(3) ?
C2 C3 . 1.385(4) ?
C2 C1 . 1.386(4) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.387(3) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.382(3) ?
C4 H4 . 0.9500 ?
C5 H5 . 0.9500 ?
N11 C15 . 1.344(3) ?
N11 C11 . 1.346(3) ?
C11 C12 . 1.382(3) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.389(4) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.378(4) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.387(3) ?
C14 H14 . 0.9500 ?
C15 H15 . 0.9500 ?
C1 H1 . 0.9500 ?
N21 C25 . 1.333(4) ?
N21 C21 . 1.337(3) ?
C21 C22 . 1.379(4) ?
C21 H21 . 0.9500 ?
C22 C23 . 1.386(5) ?
C22 H22 . 0.9500 ?
C23 C24 . 1.368(4) ?
C23 H23 . 0.9500 ?
C24 C25 . 1.379(4) ?
C24 H24 . 0.9500 ?
C25 H25 . 0.9500 ?
N30 C30 . 1.087(4) ?
C30 N31 . 1.360(4) ?
N31 C30 2_765 1.360(4) ?
