#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (vie 19 de feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/64/2016475.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_2016475
loop_
_publ_author_name
'Pagola, Silvina'
'Pike, Robert D.'
'deKrafft, Kathryn'
'Tronic, Tristan A.'
_publ_section_title
;
 Poly[μ-2-aminopyrazine-κ²N¹:N⁴-μ-cyanido-copper(I)]:
 a three-dimensional network from laboratory powder diffraction data
;
_journal_coeditor_code           FA3122
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m134
_journal_page_last               m136
_journal_paper_doi               10.1107/S010827010800231X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Cu (C1 N1) (C4 H5 N3)]'
_chemical_formula_moiety         'C5 H5 Cu N4'
_chemical_formula_sum            'C5 H5 Cu N4'
_chemical_formula_weight         184.68
_chemical_name_systematic
;
Poly[μ-2-aminopyrazine-κ²N¹:N⁴-μ-cyanido-copper(I)]
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   11.536(1)
_cell_length_b                   6.7868(7)
_cell_length_c                   8.3073(9)
_cell_measurement_pressure       101
_cell_measurement_temperature    298
_cell_volume                     650.40(11)
_computing_cell_refinement       'GSAS (Larson & Von Dreele, 2000)'
_computing_data_collection       'Philips X'Pert Data Collector Software'
_computing_data_reduction        'GSAS (Larson & Von Dreele, 2000)'
_computing_molecular_graphics
;
Mercury (Version 1.4.2; Macrae et al.,  2006)
;
_computing_publication_material
;
publCIF (Version 1.5.1_c_beta; Westrip, 2008)
;
_computing_structure_refinement  'GSAS (Larson & Von Dreele, 2000)'
_computing_structure_solution
;
EXPO2004 (Altomare et al.,  2004) and PSSP (Stephens & Pagola,
unpublished results)
;
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'Philips Analytical X'Pert Pro MRD'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_max       9
_exptl_absorpt_coefficient_mu    4.068
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_F_000             368.0
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  yellow
_pd_char_particle_morphology     'fine powder'
_pd_meas_2theta_range_inc        0.025
_pd_meas_2theta_range_max        135.00
_pd_meas_2theta_range_min        14.00
_pd_meas_scan_method             step
_pd_phase_name                   CuCNPyzNH2
_pd_prep_cool_rate               0
_pd_prep_pressure                101
_pd_prep_temperature             298
_pd_proc_info_excluded_regions   none
_pd_proc_ls_pref_orient_corr
'March--Dollase as implemented in GSAS along the (111) axis'
_pd_proc_ls_profile_function
;
Pseudovoigt (Thompson <i>et al.</i>,  1987), with asymmetry correction
from Finger <i>et al.</i> (1994) and microstrain broadening as
reported by Stephens
(1999).
;
_pd_proc_ls_prof_R_factor        0.0174
_pd_proc_ls_prof_wR_expected     0.0149
_pd_proc_ls_prof_wR_factor       0.0257
_pd_proc_wavelength              1.5418
_pd_spec_mounting                'packed powder in flat plate holder'
_pd_spec_mount_mode              reflection
_pd_spec_shape                   cylinder
_pd_spec_size_axial              27
_pd_spec_size_equat              27
_pd_spec_size_thick              2
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.402
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.72
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    41
_refine_ls_number_parameters     149
_refine_ls_number_restraints     1
_refine_ls_R_I_factor            0.0834
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.00
_refine_ls_weighting_scheme      sigma
_reflns_number_total             1246
_cod_data_source_file            fa3122.cif
_cod_data_source_block           I
_cod_original_cell_volume        650.4(1)
_cod_database_code               2016475
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x+1/2,+y,+z+1/2
3 +x+1/2,-y,+z
4 -x,-y,+z+1/2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_22
_atom_site_aniso_U_23
_atom_site_aniso_U_33
Cu1 0.045(6) -0.007(7) 0.015(9) 0.032(5) -0.01(1) 0.126(9)
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Cu Cu1 0.5088(9) 0.2041(6) 0.939(6) 1.0 Uani 0.06738 4
N N2 0.160(2) 0.619(3) 0.956(7) 1.0 Uiso 0.066(7) 4
C C3 0.260(1) 0.688(2) 0.897(7) 1.0 Uiso 0.066(7) 4
C C4 0.362(2) 0.573(3) 0.907(7) 1.0 Uiso 0.066(7) 4
N N5 0.364(3) 0.397(3) 0.973(7) 1.0 Uiso 0.066(7) 4
C C6 0.263(3) 0.330(2) 1.031(7) 1.0 Uiso 0.066(7) 4
C C7 0.164(3) 0.440(3) 1.023(7) 1.0 Uiso 0.066(7) 4
N N8 0.262(1) 0.869(3) 0.831(7) 1.0 Uiso 0.066(7) 4
H H4 0.4309 0.6243 0.8657 1.0 Uiso 0.079 4
H H6 0.2603 0.2057 1.0786 1.0 Uiso 0.079 4
H H7 0.0961 0.3884 1.0655 1.0 Uiso 0.079 4
H H8A 0.1981 0.9374 0.8269 1.0 Uiso 0.079 4
H H8B 0.3242 0.9157 0.7921 1.0 Uiso 0.079 4
C C9 0.498(9) 0.01(1) 1.10621 1.0 Uiso 0.066(7) 4
N N10 0.496(5) -0.075(6) 1.227(5) 1.0 Uiso 0.066(7) 4
loop_
_atom_type_symbol
_atom_type_number_in_cell
N 16.0
C 20.0
H 20.0
Cu 4.0
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
C4 N5 C6 116(3) 1_555 1_555 n
C4 N5 Cu1 121(3) 1_555 1_555 n
C6 N5 Cu1 121(1) 1_555 1_555 n
N2 C7 C6 123(3) 1_555 1_555 n
C7 N2 C3 116(2) 1_555 1_555 n
C7 N2 Cu1 124(1) 1_555 3_465 n
C3 N2 Cu1 119.1(9) 1_555 3_465 n
N5 C4 C3 123(3) 1_555 1_555 n
N8 C3 N2 118.9(16) 1_555 1_555 n
N8 C3 C4 121(2) 1_555 1_555 n
N2 C3 C4 120(3) 1_555 1_555 n
N5 C6 C7 122(3) 1_555 1_555 n
N5 Cu1 N10 112(2) 1_555 4_654 n
N2 Cu1 C9 113(3) 3_565 1_555 n
N2 Cu1 N10 109(2) 3_565 4_654 n
C9 Cu1 N10 110(2) 1_555 4_654 n
N5 Cu1 N2 106.7(7) 1_555 3_565 n
Cu1 C9 N10 167(6) 1_555 1_555 n
Cu1 N10 C9 176(5) 4_655 1_555 n
N5 Cu1 C9 106(3) 1_555 1_555 n
C3 N8 H8A 120.0 1_555 1_555 n
C3 N8 H8B 120.0 1_555 1_555 n
H8A N8 H8B 120.0 1_555 1_555 n
N5 C4 H4 118.8 1_555 1_555 n
C3 C4 H4 118.8 1_555 1_555 n
N2 C7 H7 118.4 1_555 1_555 n
C6 C7 H7 118.4 1_555 1_555 n
N5 C6 H6 119.4 1_555 1_555 n
C7 C6 H6 119.4 1_555 1_555 n
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
N8 C3 1.35(4) 1_555 n
N5 C4 1.32(4) 1_555 n
N5 C6 1.34(5) 1_555 n
N5 Cu1 2.14(3) 1_555 n
C7 N2 1.34(4) 1_555 n
C7 C6 1.37(4) 1_555 n
N2 C3 1.34(4) 1_555 n
N2 Cu1 2.12(2) 3_465 n
C4 N5 1.32(4) 1_555 n
C4 C3 1.41(3) 1_555 n
Cu1 C9 1.91(8) 1_555 n
Cu1 N10 1.97(7) 4_654 n
C9 N10 1.16(5) 1_555 n
N8 H8A 0.860 1_555 n
N8 H8B 0.860 1_555 n
C7 H7 0.930 1_555 n
C4 H4 0.930 1_555 n
C6 H6 0.930 1_555 n
loop_
_pd_block_diffractogram_id
HISTOGRAM
1
HISTOGRAM
2
HISTOGRAM
4
loop_
_pd_phase_block_id
CuCNPyzNH2
