#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:26:43 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179631 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/95/4509553.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_4509553
loop_
_publ_author_name
'Jaremko, Łukasz'
'Kirillov, Alexander M.'
'Smoleński, Piotr'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Engineering Coordination and Supramolecular Copper−Organic
 Networks by Aqueous Medium Self-Assembly with
 1,3,5-Triaza-7-phosphaadamantane (PTA)
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3006
_journal_paper_doi               10.1021/cg900334w
_journal_volume                  9
_journal_year                    2009
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C6 H12 Cu N6 P'
_chemical_formula_sum            'C6 H12 Cu N6 P'
_chemical_formula_weight         262.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.30(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.543(3)
_cell_length_b                   12.190(5)
_cell_length_c                   12.043(5)
_cell_measurement_reflns_used    14020
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      42.05
_cell_measurement_theta_min      4.66
_cell_volume                     926.5(7)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'PLATON (Spek, 2003) and XP (Bruker, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Oxford Xcalibur PX κ geometry'
_diffrn_measurement_method       'ω and 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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.1202
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22496
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         42.05
_diffrn_reflns_theta_min         4.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.497
_exptl_absorpt_correction_T_max  0.81639
_exptl_absorpt_correction_T_min  0.75077
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         6307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0348
_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)+(0.0352P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                3414
_reflns_number_total             6307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg900334wsup1.cif
_cod_data_source_block           (I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4509553
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.93363(3) 0.120594(15) 0.498379(16) 0.01028(5) Uani 1 1 d .
P1 P 0.62890(6) 0.20331(3) 0.46538(3) 0.00956(8) Uani 1 1 d .
N1 N 0.3870(2) 0.38415(10) 0.48734(11) 0.0112(2) Uani 1 1 d .
N2 N 0.19916(19) 0.20613(10) 0.46660(11) 0.0093(2) Uani 1 1 d .
N3 N 0.2912(2) 0.29205(10) 0.29826(11) 0.0113(2) Uani 1 1 d .
C2 C 0.3966(2) 0.13893(12) 0.50170(13) 0.0103(3) Uani 1 1 d .
H2A H 0.3696 0.0665 0.4634 0.012 Uiso 1 1 calc R
H2B H 0.4315 0.1264 0.5858 0.012 Uiso 1 1 calc R
C6 C 0.1407(2) 0.22545(12) 0.33932(13) 0.0110(3) Uani 1 1 d .
H6A H 0.1263 0.1535 0.2999 0.013 Uiso 1 1 calc R
H6B H 0.0005 0.2618 0.3169 0.013 Uiso 1 1 calc R
C5 C 0.2330(2) 0.31601(12) 0.52357(14) 0.0113(3) Uani 1 1 d .
H5A H 0.0958 0.3553 0.5065 0.014 Uiso 1 1 calc R
H5B H 0.2814 0.3054 0.6080 0.014 Uiso 1 1 calc R
C1 C 0.6039(2) 0.34073(13) 0.52585(14) 0.0118(3) Uani 1 1 d .
H1A H 0.6460 0.3362 0.6109 0.014 Uiso 1 1 calc R
H1B H 0.7022 0.3920 0.5024 0.014 Uiso 1 1 calc R
C3 C 0.4957(2) 0.23446(13) 0.31238(13) 0.0119(3) Uani 1 1 d .
H3A H 0.5906 0.2806 0.2801 0.014 Uiso 1 1 calc R
H3B H 0.4707 0.1651 0.2681 0.014 Uiso 1 1 calc R
C4 C 0.3216(3) 0.39746(12) 0.36153(14) 0.0131(3) Uani 1 1 d .
H4A H 0.4305 0.4409 0.3375 0.016 Uiso 1 1 calc R
H4B H 0.1874 0.4394 0.3400 0.016 Uiso 1 1 calc R
N11 N 1.0663(2) 0.01034(10) 0.62530(12) 0.0147(3) Uani 1 1 d .
N21 N 1.1924(2) 0.01803(10) 0.71365(12) 0.0117(3) Uani 1 1 d .
N31 N 1.3175(2) 0.02372(13) 0.80458(13) 0.0214(3) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.00780(8) 0.00925(8) 0.01436(10) 0.00067(7) 0.00395(6) 0.00081(7)
P1 0.00736(17) 0.00851(16) 0.01338(19) 0.00053(14) 0.00377(14) 0.00029(14)
N1 0.0089(5) 0.0088(5) 0.0178(7) -0.0005(5) 0.0066(5) -0.0007(5)
N2 0.0078(5) 0.0084(5) 0.0125(6) -0.0002(4) 0.0039(4) 0.0009(5)
N3 0.0088(6) 0.0123(6) 0.0130(6) 0.0014(5) 0.0032(5) 0.0000(5)
C2 0.0083(6) 0.0097(7) 0.0131(7) 0.0015(5) 0.0033(5) -0.0001(5)
C6 0.0084(6) 0.0130(7) 0.0108(7) 0.0011(5) 0.0013(5) -0.0007(5)
C5 0.0100(6) 0.0095(6) 0.0159(8) -0.0023(5) 0.0062(5) -0.0003(5)
C1 0.0089(7) 0.0111(6) 0.0157(8) -0.0010(6) 0.0040(5) -0.0012(5)
C3 0.0109(7) 0.0124(6) 0.0140(7) -0.0007(6) 0.0059(5) 0.0004(6)
C4 0.0118(7) 0.0108(7) 0.0181(8) 0.0042(5) 0.0064(6) 0.0027(5)
N11 0.0189(7) 0.0100(6) 0.0165(7) 0.0023(5) 0.0071(5) 0.0013(5)
N21 0.0111(6) 0.0066(5) 0.0208(7) -0.0012(5) 0.0104(5) -0.0005(5)
N31 0.0161(7) 0.0268(8) 0.0199(8) -0.0029(6) 0.0022(6) -0.0026(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'
P P 0.1023 0.0942 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N11 Cu1 N2 104.38(6) . 1_655
N11 Cu1 P1 128.90(5) . .
N2 Cu1 P1 119.24(5) 1_655 .
N11 Cu1 N11 87.31(7) . 3_756
N2 Cu1 N11 95.03(6) 1_655 3_756
P1 Cu1 N11 112.30(5) . 3_756
C1 P1 C3 97.95(7) . .
C1 P1 C2 97.28(7) . .
C3 P1 C2 96.93(8) . .
C1 P1 Cu1 121.30(6) . .
C3 P1 Cu1 116.32(6) . .
C2 P1 Cu1 121.83(6) . .
C5 N1 C1 112.72(12) . .
C5 N1 C4 109.56(13) . .
C1 N1 C4 111.03(12) . .
C2 N2 C5 110.46(12) . .
C2 N2 C6 110.13(12) . .
C5 N2 C6 107.21(11) . .
C2 N2 Cu1 111.32(9) . 1_455
C5 N2 Cu1 112.48(9) . 1_455
C6 N2 Cu1 105.02(9) . 1_455
C6 N3 C4 108.65(12) . .
C6 N3 C3 111.55(12) . .
C4 N3 C3 110.95(12) . .
N2 C2 P1 113.64(10) . .
N2 C2 H2A 108.8 . .
P1 C2 H2A 108.8 . .
N2 C2 H2B 108.8 . .
P1 C2 H2B 108.8 . .
H2A C2 H2B 107.7 . .
N3 C6 N2 114.94(12) . .
N3 C6 H6A 108.5 . .
N2 C6 H6A 108.5 . .
N3 C6 H6B 108.5 . .
N2 C6 H6B 108.5 . .
H6A C6 H6B 107.5 . .
N1 C5 N2 113.78(12) . .
N1 C5 H5A 108.8 . .
N2 C5 H5A 108.8 . .
N1 C5 H5B 108.8 . .
N2 C5 H5B 108.8 . .
H5A C5 H5B 107.7 . .
N1 C1 P1 112.32(11) . .
N1 C1 H1A 109.1 . .
P1 C1 H1A 109.1 . .
N1 C1 H1B 109.1 . .
P1 C1 H1B 109.1 . .
H1A C1 H1B 107.9 . .
N3 C3 P1 112.58(11) . .
N3 C3 H3A 109.1 . .
P1 C3 H3A 109.1 . .
N3 C3 H3B 109.1 . .
P1 C3 H3B 109.1 . .
H3A C3 H3B 107.8 . .
N1 C4 N3 113.43(12) . .
N1 C4 H4A 108.9 . .
N3 C4 H4A 108.9 . .
N1 C4 H4B 108.9 . .
N3 C4 H4B 108.9 . .
H4A C4 H4B 107.7 . .
N21 N11 Cu1 133.39(11) . .
N21 N11 Cu1 123.65(11) . 3_756
Cu1 N11 Cu1 92.69(7) . 3_756
N11 N21 N31 178.17(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N11 2.0484(15) .
Cu1 N2 2.1455(14) 1_655
Cu1 P1 2.1753(10) .
Cu1 N11 2.1832(15) 3_756
P1 C1 1.8509(17) .
P1 C3 1.8578(18) .
P1 C2 1.8626(16) .
N1 C5 1.459(2) .
N1 C1 1.470(2) .
N1 C4 1.471(2) .
N2 C2 1.493(2) .
N2 C5 1.4946(19) .
N2 C6 1.497(2) .
N3 C6 1.459(2) .
N3 C4 1.480(2) .
N3 C3 1.481(2) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
N11 N21 1.166(2) .
N21 N31 1.183(2) .
