#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/69/2236966.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_2236966
loop_
_publ_author_name
'Díaz, Jesús García'
'Albor, Atzimba García'
'Jaime, Espino Valencia'
'Vrábel, Viktor'
'Kožíšek, Jozef'
_publ_section_title
;
 Poly[diamminedi-μ₃-dicyanamido-copper(II)]
;
_journal_coeditor_code           LR2087
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i89
_journal_page_last               i90
_journal_paper_doi               10.1107/S1600536812045382
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu (C2 N3)2 (N H3)2]'
_chemical_formula_moiety         'C4 H6 Cu N8'
_chemical_formula_sum            'C4 H6 Cu N8'
_chemical_formula_weight         229.72
_chemical_name_systematic
;
Poly[diamminedi-μ₃-dicyanamido-copper(II)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 113.782(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.1310(2)
_cell_length_b                   9.6301(2)
_cell_length_c                   7.2162(2)
_cell_measurement_reflns_used    15460
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.2836
_cell_measurement_theta_min      3.7338
_cell_volume                     453.47(2)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2010)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1998)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10.4340
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R CCD'
_diffrn_measurement_method       'ω and φ 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  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0044
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            19836
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.74
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.376
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis RED (Oxford Diffraction, 2010), based on expressions derived
by
Clark & Reid (1995)]
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             230
_exptl_crystal_size_max          0.5215
_exptl_crystal_size_mid          0.3168
_exptl_crystal_size_min          0.1680
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0170
_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)+(0.0314P)²+0.1130P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0521
_reflns_number_gt                1019
_reflns_number_total             1126
_reflns_threshold_expression     I>2sigma(I)
_iucr_refine_instructions_details
;
TITL  P21/c
CELL  0.71073  7.1310  9.6301  7.2162 90.00000 113.782 90.00000
ZERR 4  0.0002  0.0002  0.0002  0.00000  0.00300  0.00000
LATT 1
SYMM -X, Y+ 0.50000, -Z+ 0.50000
SFAC C H N CU
UNIT 8 12 16 2
L.S. 12
PLAN  -15
MORE 3
LIST 4
SHEL 8.0 0.75
CONF
FMAP 2
ACTA 50
EQIV $1 x-1, -y+1/2, z-1/2
EQIV $2 -x, y+1/2, -z+3/2
EQIV $3 -x, -y, -z+1
HTAB N1 N4_$1
HTAB N1 N4_$2
HTAB N1 N4_$3
HTAB
BOND $H
MERG 2
WGHT    0.031400    0.113000
FVAR      10.71916
C1    1    0.125004    0.206155    0.407366    11.00000    0.03491    0.02847 =
         0.02926   -0.00341    0.01142    0.00081
C2    1    0.256702   -0.007037    0.516775    11.00000    0.03398    0.02705 =
         0.03322   -0.00556    0.01395   -0.00185
N1    3   -0.268488    0.416480    0.455137    11.00000    0.04052    0.02990 =
         0.03648   -0.00012    0.01382   -0.00045
H1    2   -0.351280    0.471962    0.371066    11.00000    0.05392
H2    2   -0.283344    0.416953    0.571611    11.00000    0.05293
H3    2   -0.281366    0.338435    0.410391    11.00000    0.06175
N2    3    0.090271    0.321100    0.420577    11.00000    0.05181    0.02759 =
         0.04306   -0.00420    0.01679    0.00538
N3    3    0.151069    0.077721    0.368791    11.00000    0.05197    0.02667 =
         0.03134   -0.00463    0.00974    0.00767
N4    3    0.345971   -0.090507    0.634059    11.00000    0.05198    0.03531 =
         0.04588    0.00449    0.01397    0.00330
CU1   4    0.000000    0.500000    0.500000    10.50000    0.03572    0.01832 =
         0.03050   -0.00132    0.01271    0.00135
HKLF 4
REM   P21/c
REM R1 =  0.0170 for   1019 Fo > 4sig(Fo)  and  0.0194 for all   1126 data
REM     74 parameters refined using      0 restraints
END
;
_cod_data_source_file            lr2087.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2236966
_cod_database_fobs_code          2236966
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
C C1 0.12500(18) 0.20615(12) 0.40737(17) 0.0314(2) Uani d . 1 1
C C2 0.2567(2) -0.00704(11) 0.5168(2) 0.0313(3) Uani d . 1 1
N N1 -0.26849(18) 0.41648(13) 0.45514(19) 0.0362(2) Uani d . 1 1
H H1 -0.351(3) 0.472(2) 0.371(4) 0.054(6) Uiso d . 1 1
H H2 -0.283(3) 0.417(2) 0.572(3) 0.053(5) Uiso d . 1 1
H H3 -0.281(3) 0.338(3) 0.410(3) 0.062(6) Uiso d . 1 1
N N2 0.09027(19) 0.32110(12) 0.42058(18) 0.0416(3) Uani d . 1 1
N N3 0.15107(18) 0.07772(11) 0.36879(16) 0.0389(3) Uani d . 1 1
N N4 0.3460(2) -0.09051(13) 0.63406(19) 0.0462(3) Uani d . 1 1
Cu Cu1 0.0000 0.5000 0.5000 0.02839(10) Uani d S 1 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0349(5) 0.0285(6) 0.0293(5) 0.0008(4) 0.0114(4) -0.0034(4)
C2 0.0340(6) 0.0271(6) 0.0332(6) -0.0019(4) 0.0140(5) -0.0056(4)
N1 0.0405(6) 0.0299(5) 0.0365(6) -0.0005(4) 0.0138(5) -0.0001(5)
N2 0.0518(7) 0.0276(5) 0.0431(6) 0.0054(5) 0.0168(5) -0.0042(4)
N3 0.0520(6) 0.0267(5) 0.0313(5) 0.0077(4) 0.0097(5) -0.0046(4)
N4 0.0520(7) 0.0353(6) 0.0459(6) 0.0033(5) 0.0140(5) 0.0045(5)
Cu1 0.03572(14) 0.01832(13) 0.03050(14) 0.00135(6) 0.01271(10) -0.00132(6)
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'
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
N2 C1 N3 . . 172.98(14)
N4 C2 N3 . . 173.97(14)
Cu1 N1 H1 . . 102.1(15)
Cu1 N1 H2 . . 108.6(12)
H1 N1 H2 . . 111(2)
Cu1 N1 H3 . . 112.9(15)
H1 N1 H3 . . 112(2)
H2 N1 H3 . . 110.2(19)
C1 N2 Cu1 . . 163.67(11)
C1 N3 C2 . . 120.18(11)
N1 Cu1 N1 3_566 . 180.00(7)
N1 Cu1 N2 3_566 . 89.72(5)
N1 Cu1 N2 . . 90.28(5)
N1 Cu1 N2 3_566 3_566 90.28(5)
N1 Cu1 N2 . 3_566 89.72(5)
N2 Cu1 N2 . 3_566 180.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N2 . 1.1466(17)
C1 N3 . 1.2975(16)
C2 N4 . 1.1546(18)
C2 N3 . 1.3135(17)
N1 Cu1 . 1.9793(12)
N1 H1 . 0.84(2)
N1 H2 . 0.89(2)
N1 H3 . 0.81(2)
N2 Cu1 . 2.0021(11)
Cu1 N1 3_566 1.9793(12)
Cu1 N2 3_566 2.0021(11)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1 N4 4_465 0.84(2) 2.43(2) 3.2555(18) 165.4(19)
N1 H2 N4 2_556 0.89(2) 2.34(2) 3.2278(18) 175.7(17)
N1 H3 N4 3_556 0.81(2) 2.43(2) 3.2073(18) 162.1(19)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_4
_geom_torsion
N3 C1 N2 Cu1 . 124.8(10)
N2 C1 N3 C2 . -178.5(11)
N4 C2 N3 C1 . 18E1(10)
C1 N2 Cu1 N1 3_566 130.8(4)
C1 N2 Cu1 N1 . -49.2(4)
C1 N2 Cu1 N2 3_566 2E1(10)
